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There is great concern in equine sport over the potential use of pharmaceutical agents capable of editing the genome or modifying the expression of gene products. Synthetic oligonucleotides are short, single-stranded polynucleotides that represent a class of agents capable of modifying gene expression products with a high potential for abuse in horseracing. As these substances are not covered by most routine anti-doping analytical approaches, they represent an entire class of compounds that are not readily detectable. The nucleotide sequence for each oligonucleotide is highly specific, which makes targeted analysis for these agents problematic. Accordingly, we have developed a non-targeted approach to detect the presence of specific product ions that are not naturally present in ribonucleic acids. Briefly, serum samples were extracted using solid-phase extraction with a mixed-mode cartridge following the disruption of protein interactions to isolate the oligonucleotides. Following the elution and concentration steps, chromatographic separation was achieved utilizing reversed-phase liquid chromatography. Following an introduction to a Thermo Q Exactive HF mass spectrometer using electrospray ionization, analytes were detected utilizing a combination of full-scan, parallel reaction monitoring and all ion fragmentation scan modes. The limits of detection were determined along with the accuracy, precision, stability, recovery, and matrix effects using a representative 13mer oligonucleotide. Following method optimization using the 13mer oligonucleotide, the method was applied to successfully detect the presence of specific product ions in three unique oligonucleotide sequences targeting equine-specific transcripts.

Therapeutic drug monitoring is essential for ensuring the efficacy and safety of medications. This study introduces a streamlined approach that combines pipette-tip solid-phase extraction (PT-SPE) with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), facilitating rapid and high-throughput monitoring of drug concentrations. As a demonstration, this method was applied to the extraction and quantification of antidepressants in serum. Utilizing Zip-Tip C18, the method enabled the extraction of antidepressants from complex biological matrices in less than 2 min, with the subsequent MALDI-MS analysis yielding results in just 1 min. Optimal extraction recoveries were achieved using a sampling solution at pH 9.0 and a 10 μL ethanol desorption solution containing 0.1% phosphoric acid. For MALDI analysis, 2,5-dihydroxybenzoic acid was identified as the most effective matrix for producing the highest signal intensity. The quantification strategy exhibited robust linearities (R2 ≥ 0.997) and satisfactory limits of quantification, ranging from 0.05 to 0.5 μg/mL for a suite of antidepressants. The application for monitoring dynamic concentration changes of antidepressants in rat serum emphasized the method's efficacy. This strategy offers the advantages of high throughput, minimal sample usage, environmental sustainability, and simplicity, providing ideas and a reference basis for the subsequent development of methods for therapeutic drug monitoring. [ABSTRACT FROM AUTHOR]

AbstractMethiocarb is a carbamate pesticide and is widely used due to its short lifetime but is a health concern due to its toxicity. To address this challenge, a novel nano-sorbent (zinc aluminate hybrid doped onto a magnetic activated carbon cloth (magnetic ACC@ZnAl2O4)) was synthesized. The characterization of the composite was done using FTIR spectroscopy, SEM, XRD, and EDX. The synthesized composite was then employed for the efficient extraction of methiocarb from food samples. Under the optimum conditions of (pH: 7.0, vortex time: 0.5 min, adsorbent dose: 5 mg, initial volume of sample: 50 mL, volume of eluent: 1.0 mL), quantitative recovery values of methiocarb in food samples were obtained (80–114%). This method impresses with its exceptional sensitivity, achieving incredibly low detection (LOD: 20 µg L−1) and quantification (LOQ: 67 µg L−1) limits for methiocarb. Its efficiency is equally impressive, with high values of preconcentration factor (PF: 50) and enhancement factor (EF: 49.4), ensuring accurate and reliable analysis with a low value of relative standard deviation (RSD: 4.8%). The method’s impressive selectivity, evident in its minimal interference from other pesticides, paves the way for reliable methiocarb analysis in food samples. [ABSTRACT FROM AUTHOR]

Xylazine has emerged in recent years as a dangerous adulterant in illicit fentanyl use, and methods for the detection of xylazine in toxicology panels are still lagging. We developed methods for the screening and quantitation of xylazine in oral fluid (OF), a popular testing medium due to its ease of collection and reflection of presence in blood for many classes of drugs. Enzyme-linked immunosorbent assays were employed for the rapid screening of xylazine directly from the collection device buffer with a cutoff of 1 ng/mL. Solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry facilitated the confirmation and quantification of xylazine as low as 0.1 ng/mL and a dynamic range of 0.1–25 ng/mL. Selectivity, ionization suppression, processed sample stability, and dilution effect were also assessed. The method was validated through the American National Standards Institute/American Academy of Forensic Sciences Standards Board (ANSI/ASB) Standard 036, first edition from 2019, and found to be accurate, precise, and robust. Living human subject OF samples collected within substance use disorder and therapeutic drug monitoring clinics received between September 2023 and January 2024, with the specific request to test for xylazine (n  = 57), were screened. Presumptive positive samples were confirmed using the validated method. Xylazine confirmed living human subject OF sample concentrations ranged from 1.2 to 23.3 ng/mL. [ABSTRACT FROM AUTHOR]

This review article describes some of the recent advances in ultra‐trace determination of uranium in various natural water bodies such as drinking water, underground water, seawater, etc. using total reflection x‐ray florescence (TXRF) spectrometry. Uranium is one of the most hazardous element having chemical as well as radio‐toxicity. However, due to its low concentration in water samples, direct determination is seldom possible in samples with high salt content. Various sample preconcentration and selective extraction techniques for uranium such as solvent extraction, dispersive liquid–liquid micro extraction, solid phase extraction, and membrane based preconcentration methods are summarized in this article. TXRF is a very versatile micro‐analytical technique with detection limits in picogram range and having multielemental analysis capability. TXRF determination of uranium using U Lα as the analytical line has many analytical challenges and difficulties, mainly due to the severe interference with Rb and Br, both are commonly available in natural water samples. This article highlights some of these challenges, along with the advantages and disadvantages of the different sample preparation techniques used so far for uranium determination in natural water samples by TXRF. [ABSTRACT FROM AUTHOR]

The applicability of two layered double hydroxide adsorbents, that is, Zn/Al LDH and the reduced graphene oxide-modified Zn/Al-rGO LDH for the solid phase extraction-preconcentration of naproxen followed by HPLC determination is evaluated and compared. The adsorbents are characterized by using XRD, FT-IR, FE-SEM, BET, and TEM techniques. The optimization of parameters affecting the extraction procedure included pH and sample solution volume, amount of the adsorbents, adsorbent/sample solution contact time, type, concentration, and volume of the desorption solution, and the time required for desorption process was performed by using univariate method. It is assumed that the uptake of anionic form of naproxen is taken place via the ion exchange mechanism with interlayer carbonate anions of the studied LDHs. The applicability of the adsorbents is evaluated by the determination of naproxen in human urine, hospital, and pharmaceutical wastewater samples. The obtained linear ranges by employing the unmodified and modified LDHs for the determination of naproxen in pharmaceutical wastewater were found to be 10–530 µg L−1 (R2 = 0.9999) and 5–630 µg L−1 (R2 = 0.9999), respectively. The limits of detection and enrichment factor were appraised as 5.1 µg L−1 and 42 by employing Zn/Al LDH, and 3.1 µg L−1 and 54.5 by using Zn/Al-rGO LDH. Both investigated LDHs are able to be used in solid phase extraction-preconcentration of naproxen in real samples. However, the evaluated figures of merit reveal that the modified Zn/Al-rGO LDH is more efficient adsorbent than the unmodified Zn/Al LDH for the extraction of naproxen. [ABSTRACT FROM AUTHOR]

Matrix effects are a major concern in liquid chromatography coupled to tandem mass spectrometry for the determination of pesticide residues. In this work, a novel and efficient lipophilicity-matched chromatographic separation strategy was developed to improve the separation efficiency on an alkyl bonded phase chromatographic column and reduce matrix effects. An ultra-high performance liquid chromatography-tandem mass spectrometry method based on this strategy was established to minimize matrix effects for the determination of triazole fungicides. The samples were cleaned-up with dispersive solid phase extraction and separated on a chromatographic column with similar lipophilicity to the fungicides. The results showed that the proposed method effectively minimized the matrix effects and improved the separation. The matrix effects of 21 fungicides ranged from −8.3% to 4.7%. Moreover, the average recoveries were between 91.4% and 108.1% using solvent calibration for quantification, and the limits of quantitation were between 0.5 and 3.5 μg/kg. These results demonstrate the effectiveness of the proposed strategy in improving the chromatographic efficiency. This work provides a practical strategy and reference for the liquid chromatography-tandem mass spectrometry determination of pesticide residues. [ABSTRACT FROM AUTHOR]

A rapid and effective method utilizing ultrasonic assisted-dispersive solid-phase microextraction coupled with gas chromatography/mass spectrometry (GC/MS) was developed for the determination of lorazepam and diazepam in biological and aqueous samples. A modified nanocrystalline cellulose-based sorbent was prepared and applied for the microextraction of the analytes. The extraction efficiency of the sorbents prepared using self-assembled N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, including cellulose nanostructure and modified nanocrystalline cellulose, was compared. The modified cellulose nanostructure was characterized using thermogravimetric analysis (TGA), energy dispersive X-ray (EDX), and Fourier transform infrared spectroscopy (FTIR). Additionally, the study investigated the effects of relevant factors on the extraction/desorption performance, including extraction time, ionic strength, and the type and volume of the desorption solvent. The method achieved limits of detection of 1 ng mL−1 and 3 ng mL−1 and quantification limits of 4 ng mL−1 and 10 ng mL−1 for lorazepam and diazepam, respectively. Furthermore, the developed method demonstrated good repeatability with relative standard deviations of 4% and 6% (n = 5) for the spiked analyte aqueous solutions at 50 ng mL−1. The method also exhibited high linearity (R > 0.9996) in the range from 10 to 1000 ng mL−1. [ABSTRACT FROM AUTHOR]

We measured the intracellular concentrations of tenofovir-diphosphate (TFV-DP) and emtricitabine-triphosphate (FTC-TP) in dried blood spots (DBS) for pre-exposure prophylaxis (PrEP) adherence using sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS). A total of 191 DBS were obtained from 85 participants who were receiving tenofovir disoproxil fumarate (TDF; 300 mg) and emtricitabine (FTC; 200 mg) as PrEP at the Sexual Health Clinic, National Center for Global Health and Medicine, Tokyo, Japan. DBS punch (3 mm) added to 25 μL of 50% methanol and 400 μL of internal standard solution was used for solid phase extraction. Chromatographic separation was achieved on an Atlantis Premier BEH C18 AX Column (50 mm × 2.1 mm i.d.; particle size 1.7 μm) using gradient elution (flow rate: 0.6 mL/min); injection volume: 7 μL and run time: 5.5 min. Calibration curves for the two drugs were linear in the range 0.05–12.5 ng/punch. We determined the intracellular TFV-DP and FTC-TP concentrations in 191 DBS obtained from 85 patients administered with TDF and FTC as PrEP. The analytical performance data (calibration curve and QC samples) for all the analytical runs met the acceptance criteria. Intracellular concentrations of TFV-DP and FTC-TP in the DBS remained stable for at least 24 h after oral administration. A multiplex LC–MS/MS method was successfully developed for DBS, which can be useful for monitoring the levels of TFV-DP and FTC-TP in individuals receiving PrEP. [ABSTRACT FROM AUTHOR]

The three-dimensional imprinted polymeric network was synthesized via a bulk polymerization reaction in the presence of a flavonoid as a template. In this reaction, methacrylic acid (MAA) and acrylic acid (AA), tetrahydrofuran and trimethylolpropanetrimethacrylate, were used as functional monomers, porogen, and cross-linker, respectively. In this study, two kinds of molecularly imprinted polymers (MIPs) with different ratios of 1:8:40 and 1:20:80 (template: functional monomer: cross-linker) were synthesized and compared together. The related binding capacities were calculated as equal to 392.08 mg/g and 609.00 mg/g, respectively, by UV-spectrometer. The synthesized polymers have been evaluated via field emission scan electron microscopy, transmission electron microscopy, and Brunauer–Emmett–Teller techniques. High selectivity and the proper specific surface area as equal to 167.00 m2/g in MIPs-based methacrylic acid (MIPs-MAA) and 434 m2/g in MIPs-based acrylic acid (MIPs-AA) comparatively to non-imprinted molecular polymers are the privileged characteristics in this research. The MIPs provided are a good candidate for the separation of flavonoids with the solid phase extraction method. [ABSTRACT FROM AUTHOR]

An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test. [ABSTRACT FROM AUTHOR]

This study introduces a miniaturised solid-phase extraction (µ-SPE) method coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous quantification of 23 compounds, including psychoactive drugs, narcotics and their metabolites, in urine samples. The µ-SPE method, using standard laboratory equipment such as a centrifuge, was developed and validated, offering a practical and economical alternative to more traditional SPE methods. The key extraction parameters: elution solvent composition, sample and elution volumes, and sorbent mass were optimized to enhance performance. The method demonstrated high sensitivity, with detection limits between 0.06 and 0.41 ng cm−3 and quantification limits from 0.19 to 1.24 ng cm−3. The precision was confirmed with an intra-day precision ranging from 0.2% to 7.5% and an inter-day precision from 1.2% to 13.4%. Recovery rates ranged from 84.2% to 109.4%, with minimal matrix effects observed for most analytes (|ME|< 10%). The relative error remained below 5%, indicating good accuracy. The method was also evaluated in terms of greenness, practical, and analytical aspects using the WAC model. Based on the validation results, it was concluded that the developed method could be a good confirmatory method for results obtained by immunochemical tests and could also be used in both clinical analyses and forensic toxicology. [ABSTRACT FROM AUTHOR]

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Rationale: The sources and chemical compositions of organic aerosol (OA) exert a significant influence on both regional and global atmospheric conditions, thereby having far‐reaching implications on environmental chemistry. However, existing mass spectrometry (MS) methods have limitations in characterizing the detailed composition of OA due to selective ionization as well as fractionation during cold‐water extraction and solid‐phase extraction (SPE). Methods: A comprehensive MS study was conducted using aerosol samples collected on dusty, clean, and polluted days. To supplement the data obtained from electrospray ionization (ESI), a strategy for analyzing OAs collected using the quartz fiber filter directly utilizing laser desorption ionization (LDI) was employed. Additionally, the ESI method was conducted to explore suitable approaches for determining various OA compositions from samples collected on dusty, clean, and polluted days. Results: In situ LDI has the advantages of significantly reducing the sample volume, simplifying sample preparation, and overcoming the problem of overestimating sulfur‐containing compounds usually encountered in ESI. It is suitable for the characterization of highly unsaturated and hydrophobic aerosols, such as brown carbon‐type compounds with low volatility and high stability, which is supplementary to ESI. Conclusions: Compared with other ionization methods, in situ LDI helps provide a complementary description of the molecular compositions of OAs, especially for analyzing OAs in polluted day samples. This method may contribute to a more comprehensive MS analysis of the elusive compositions and sources of OA in the atmosphere. [ABSTRACT FROM AUTHOR]

BACKGROUND: This study investigated per‐ and polyfluoroalkyl substances (PFASs) in 53 fruit and vegetable samples collected from a local wholesale and retail market in Sydney and a local supermarket in Newcastle. As there is limited information about PFAS levels in vegetables on the market, this study aimed to fill this gap and assess potential risks for humans through consumption of these vegetables. METHODS: QuEChERS extraction – a solid‐phase extraction method, a portmanteau word formed from 'quick, easy, cheap, effective, rugged and safe' – followed by enhanced matrix removal–lipid cleaning and liquid chromatography–tandem mass spectrometry analysis were used to detect 30 PFASs in vegetables. RESULTS: PFOA was detected in 7 out of the 53 samples, with concentrations of 0.038–1.996 ng g−1 fresh weight; PFOS was detected in 2 samples only, with concentrations ranging from 0.132 to 0.911 ng g−1 fresh weight. PFHxS was not detected in any sample in this study. PFOA and PFOS concentrations measured in vegetables in this study constituted daily intake of 2.03 ng kg−1 body weight (BW) and 1.98 ng kg−1 BW, respectively, according to recommended daily vegetable intake and BW data from the Australian Bureau of Statistics. The most sensitive population group is girls of 4–8 years of age. These estimated exposure levels represent up to 1.3% of the tolerable daily intake for PFOA (160 ng kg−1 BW) and 9.9% for PFOS (20 ng kg−1 BW) according to Food Standards Australia New Zealand. Consumption of the vegetables from the study locations poses a marginal risk to human health. © 2024 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

This study investigates the presence of new psychoactive substances (NPS) and their metabolites in two wastewater treatment plants (WWTPs) situated in South Wales, UK (WWTP-1 and WWTP-2). Analysis was conducted for 35 NPS and metabolites, along with the inclusion of benzoylecgonine (main cocaine metabolite) and cannabis, the most detected illicit substances. Benzoylecgonine was identified as the predominant substance in both WWTPs. Epidemiological calculations revealed the average population consumption of cocaine to be 3.88 mg/d/1000 inhabitants around WWTP-1 and 1.97 mg/d/1000 inhabitants for WWTP-2. The removal efficiency of benzoylecgonine across both WWTPs was observed at an average of 73%. Subsequent qualitative analyses on randomly selected wastewater samples detected medicinal compounds including buprenorphine, methadone, and codeine in both WWTPs. An additional experiment employing enzymatic hydrolysis revealed the presence of morphine, an increased presence of codeine, and 11-Nor-9-Carboxy-THC (THC-COOH) post-hydrolysis. These findings underscore the significant presence of illicit substances and medicinal compounds in wastewater systems with the absence of NPS within the South Wales area, highlighting the necessity for enhanced monitoring and treatment strategies to address public health and environmental concerns. [ABSTRACT FROM AUTHOR]

AbstractAs an alternative to bisphenol A (BPA), bisphenol S (BPS) has been used as an ink developer in thermal paper products including price labels on food packaging which have been suggested as the sources of BPS found at high levels in packaged fish samples. BPS in the printed price labels glued onto the outside of plastic film could migrate indirectly from the printed surface through the paper, adhesive and film into the food. In order to investigate if price labels could also be the sources of BPS detected in the meat samples in our previous studies, meat and other food samples packaged under different conditions were collected, and BPS in these samples together with the price labels on the corresponding packaging were extracted with solvent followed by solid phase extraction and stable isotope dilution LC-MS/MS analysis. BPS was detected at very high levels (161.7–222.4 µg/cm2) in all the five sticker type of price labels, indicating BPS being the dominant if not the sole ink developer. BPS was also detected in all the 26 continuous roll type of price labels but at very low levels (0.017–18 ng/cm2), indicating that the dominant ink developer is likely one of the other alternatives, rather than BPS. Despite BPS being detected in all price labels on packaging of fish, meat, and cheese samples, BPS was not detected or detected in only a few fish, meat, and cheese samples at levels considerably lower than the current EU specific migration limit (SML) of 50 ng/g food for BPS authorised under Regulation (EU) 10/2011. [ABSTRACT FROM AUTHOR]

Introduction: The presence of pharmaceuticals and personal care products in environmental matrices is considered one of the major scientific concerns. Most of these substances are disposed of unchanged through wastewater treatment plants and sewage systems. Consequently, they are continuously introduced into the water systems and progressively contaminate surface, ground and drinking water. During the COVID-19 pandemic, a large number of emerging contaminants including parabens were released to the environment through various routes. In this study, the occurrence of parabens (methylparaben (MePB), ethylparaben (EtPB), propylparaben (PrPB), and butylparaben (BuPB) was investigated in wastewater samples from various wastewater treatment plants (WWTPs) and the receiving surface waters in KwaZulu Natal and Gauteng Provinces (South Africa). Methods: The samples were collected between October 2020 and December 2021, covering the 2nd, 3rd and 4th waves of the COVID-19 pandemic. A solid phase extraction protocol with high-performance liquid chromatography was used to extract and enrich parabens before analysis. Results and Discussion: Methylparaben (2.02-84.7 μg/L), EtPB (<0.24-24.8 μg/L), PrPB (<0.26-55.1 μg/L), and BuPB (<0.27-17.3 μg/L) were quantified in wastewater influent collected WWTPs of KwaZulu Natal Province. While <0.19-5.43 μg/L, <0.16-5.63 μg/L, <0.17-6.89 μg/L, and <0.19-5.32 μg/L for MePB, EtPB, PrPB, and BuPB, respectively, were quantified in effluent wastewater from the same province. The concentrations of MePB, EtPB, PrPB, and BuPB in influent wastewater from Gauteng Province were 2.58-123 μg/L, <0.24-33.6 μg/L, 3.77-73.4 μg/L and <0.27-85.8 μg/L, respectively. In effluent wastewater, concentrations ranging from 0.24-17.76 μg/L (MePB), <0.16-4.88 μg/L (EtPB), 0.69-12.5 μg/L (PrPB), and <0.19-4.726 μg/L (BuPB) were quantified. During the 4th wave, the concentrations of parabens in surface water were lower compared to the second and third waves of the pandemic. In general, the paraben residues in the surface of KwaZulu Natal Province (<0.08-16.4 μg/L) were higher than those in Gauteng Province (0.08-3.14 µg/L). Methylparaben and propylparaben were dominant in all investigated samples (wastewater and surface water), followed by ethylparaben. The ecotoxicological risk assessment was carried out for aquatic biota, which was estimated in terms of risk quotients (RQs). RQs for the target compounds in river water indicated that MePB and EtPB pose low risk, whereas PrPB and BuPB pose low to medium risk to aquatic organisms. [ABSTRACT FROM AUTHOR]

In this study, the levels of six PAEs [bis (2-ethylhexyl) phthalate (DEHP), butyl benzyl phthalate (BBP), dibutyl phthalate (DBP), diethyl phthalate (DEP), dimethyl phthalate (DMP) and di-n-octyl phthalate (DNOP)] were determined from four types of bottled water)non-carbonated, mineral, carbonated and carbonated flavoured) using MSPE method (magnetic solid phase extraction) and GC/MS technique (gas chromatography/mass spectrometry). The mean concentration of total PAEs was 6.11 ± 1.43 µg/L. The mean concentration of DEHP was 2.22 ± 0.76 µg/L and was lower than the United States Environmental Protection Agency (USEPA) standard level in drinking water (6 μg/L for DEHP). The highest mean level of total PAE was observed in carbonated water (7.43 ± 2.03 μg/L) and the lowest mean level of total PAE was observed in non-carbonated water (5.15 ± 0.41 μg/L). The Monte Carlo method was applied to calculate the Target Hazard Quotient (THQ), Chronic Daily Intake (CDI), and Incremental Life Cancer Risk (ILCR) indexes. In all samples, the rank order of the estimated THQ values based on the 95% percentile was DEHP (4.77E-4) > DBP (2.25E-5) > BBP (1.99E-5) > DEP (2.75E-6) and there would be unlikely non-carcinogenic risks for consumers (THQ<1). The incremental lifetime cancer risk assessment revealed that phthalate esters (DEHP) in evaluated bottled water samples did not pose a serious concern to humans. [ABSTRACT FROM AUTHOR]

In the United States, illicit fentanyl is often trafficked as blue tablets mimicking the legitimate M‐30 oxycodone tablet produced by Mallinckrodt. The analysis of dyes extracted from seized fentanyl tablets could provide a useful tool for law enforcement to establish linkages between cases and could prove useful for attributing a seizure to a given trafficking organization. Fentanyl tablet seizures associated with a particular drug trafficking organization (DTO), either through investigative or intelligence information, were used as the sample set for this study. The blue dye from the tablets was isolated by solid phase extraction and then qualitatively and quantitatively analyzed via ultraviolet‐visible spectroscopy. This research revealed that the illicit tableting facilities use a different dye than several known pharmaceutical companies. The concentration of dye in individual tablets within a seizure proved to be very minimal, and the small sample size made it difficult to draw linkages from case to case. Analysis of the dyes could not effectively differentiate between the drug trafficking organizations in the tested population due to each DTO using the same dye; however, it is important to note that the dye found was consistent between illicit tablets. [ABSTRACT FROM AUTHOR]

Bisphenols are widely used as monomers and additives in plastic production. Thus, bisphenol A (BPA) and its most prominent substitutes have been detected in many environmental and human samples. This study proposes an online solid-phase extraction analytical methodology coupled to liquid chromatography with tandem mass spectrometry for the determination of six bisphenols (BPA and bisphenols F (BPF), S (BPS), AF (BPAF), B (BPB), and E (BPE)) in urine samples as an efficient and automated methodology. The method was developed and validated for all bisphenols with good recoveries (92–112%) and repeatability (RSD ≤ 10%) despite the variable matrix effects, except BPAF (which would require a dedicated internal standard), achieving method quantification limits in the 0.05–2.2 ng mL−1 range. The methodology was subsequently applied to 435 urine samples from a non-occupational exposure population (civil servants for the regional government) from Santiago de Compostela (Galicia, Spain). Only BPA, BPF, and BPS were positively detected; the last two presented higher detection frequencies than BPA. When the urinary concentrations are extrapolated to human intake and compared to the European Food Safety Agency (EFSA) tolerable daily intake (TDI) of 2 × 10−4 µg kg−1 day−1 (TDI), all BPA positively identified samples would surpass this threshold. Although no TDI exists currently for the other two identified bisphenols, it is evident that human exposure to bisphenols should be limited. Finally, the results stratification by gender revealed higher levels of exposure to BPF in the women group. [ABSTRACT FROM AUTHOR]

Antimicrobial resistance (AMR) is one of the most alarming global public health challenges of the 21st century. Over 3 million antimicrobial-resistant infections occur in the United States annually, with nearly 50,000 cases being fatal. Innovations in drug discovery methods and platforms are crucial to identify novel antibiotics to combat AMR. We present the isolation and characterization of potentially novel antibiotic lead compounds produced by the cross-feeding of two rhizosphere bacteria, Acinetobacter sp. RIT 592 and Exiguobacterium sp. RIT 594. We used solid-phase extraction (SPE) followed by liquid chromatography (LC) to enrich antibiotic extracts and subsequently mass spectrometry (MS) analysis of collected fractions for compound structure identification and characterization. The MS data were processed through the Global Natural Product Social Molecular Networking (GNPS) database. The supernatant from RIT 592 induced RIT 594 to produce a cocktail of antimicrobial compounds active against Gram-positive and negative bacteria. The GNPS analysis indicated compounds with known antimicrobial activity in the bioactive samples, including oligopeptides and their derivatives. This work emphasizes the utility of microbial community-based platforms to discover novel clinically relevant secondary metabolites. Future work includes further structural characterization and antibiotic activity evaluation of the individual compounds against pathogenic multidrug-resistant (MDR) bacteria. [ABSTRACT FROM AUTHOR]

An alternative solid phase extraction (SPE) material, 1‐butyl‐3‐methylimidazolium chloride–silver nanoparticles/eggshell membrane ([BMIM]Cl‐AgNPs/ESM), is developed by synthesizing [BMIM]Cl‐AgNPs using a simple reduction method and immobilizing directly on ESM. The newly developed material is successfully applied for extraction and detection of sulfamethoxazole (SMX) in environmental aqueous samples via a high‐performance liquid chromatography‐diode array detector (HPLC‐DAD). Characterization is accomplished by Fourier transform infrared (FTIR) and field emission scanning electron microscopy/energy dispersive X‐ray (FESEM/EDX), confirming the presence of [BMIM]Cl‐AgNPs on ESM. The optimization of [BMIM]Cl‐AgNPs/ESM‐based SPE method is studied by the one variable at a time (OVAT) approach. Method validation shows good linearity (R2 = 0.9995) in the range of 10–500 µg L−1, with the detection and quantification limits determined to be 3.07 and 9.31 µg L−1 respectively. Additionally, a reusability study shows the developed material can extract SMX up for three cycles without significant reduction in its efficiency. Excellent recoveries (90.07–104.08%) in spiked tap and lake water demonstrate the potential of [BMIM]Cl‐AgNPs/ESM for trace‐level detection of pollutants. [ABSTRACT FROM AUTHOR]

In order to investigate the mechanism of plant growth promoting (PGP) effects of strain Bacillus velezensis WSW007, its PGP traits and production of volatile organic compounds (VOCs) were tested. The effects of VOCs produced by strain WSW007 on plant growth were observed by co-culturing this strain with tobacco seedlings in I-plates. Meanwhile, the effects of VOCs on tobacco gene expression were analysed by a transcriptome analysis and VOCs were identified by solid phase micro extraction coupled with gas chromatography-mass spectrometry (SPME-GC-MS) analysis. As results, strains WSW007 produced acetic acid and siderophore, and could solubilize phosphate; while it also significantly increased the fresh weight of tobacco seedlings via production of VOCs. In transcriptome analysis, plants co-cultured with strain WSW007 presented the highest up-regulated expression for the genes involved in plant growth and development processes, implying that the bacterial VOCs played a role as regulator of plant gene expression. Conclusively, the up-regulation in expression of growth- and development-related genes via VOCs production is an important PGP mechanism in strain B. velezensis WSW007. [ABSTRACT FROM AUTHOR]

An automated flow analysis-solid phase extraction (FA-SPE) system and methodology of ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) analysis were developed for the determination of selected antiviral drugs (acyclovir, amantadine, rimantadine, and oseltamivir) in water samples. The proposed FA-SPE approach enables the integration of various extraction stages and elimination of the sample evaporation step and offers individual customisation of SPE parameters, inter alia sample, and eluate flow rate and volume. Using the developed FA-SPE procedure, e.g. a 100-fold preconcentration of the target analytes in 1 h was achieved. A method for chromatographic analysis was also developed to determine the selected antiviral drugs in combination with the use of the FA-SPE system. The developed FA-SPE UHPLC-MS/MS method was validated including the determination of linearity of analytical graphs, limits of detection (5.5–99.9 pg mL−1) and quantification (18.3–329.8 pg mL−1), intra-day (1.8–8.3%) and inter-day (3.0–9.2%) precision, recovery (95.6–105.3%), and matrix effects (− 12.9 to 13.2%). The proposed method was successfully applied to analyse tap, drinking, and river water samples, revealing the presence of amantadine at a concentration of 40.1 pg mL−1 in one sample. The environmental impact of the developed FA-SPE sample preparation procedure was also assessed using the AGREEprep metric tool and compared with five other literature methods, achieving the most sustainable outcome. [ABSTRACT FROM AUTHOR]

• Water samples extracted by different SPE methods showed distinct biotoxicities. • Biotoxicity outcomes of extracted water samples were proportional to the chemical extracting efficiencies of SPE methods. • HLB+Coconut ranked as the Pareto best for biotoxicity assessment among 5 SPE methods. • Biotoxicity outcomes and chemical extracting efficiencies synchronously decrease with increasing SVPC during SPE. Biotoxicity assessment results of environmental waters largely depend on the sample extraction protocols that enrich pollutants to meet the effect-trigger thresholds of bioassays. However, more chemical mixture does not necessarily translate to higher combined biotoxicity. Thus, there is a need to establish the link between chemical extracting efficiency and biotoxicity outcome to standardize extraction methods for biotoxicity assessment of environmental waters. This study compares the performance of five different extraction phases in solid phase extraction (SPE), namely HLB, HLB+Coconut, C18 cartridge, C18 disk and Strata-X, and evaluated their chemical extracting efficiencies and biotoxicity outcomes. We quantitatively assessed cytotoxicity, acute toxicity, genotoxicity, estrogenic activity, and neurotoxicity of the extracts using in vitro bioassays and characterized the chemical extracting efficiencies of the SPE methods through chemical recoveries of 23 model compounds with different polarities and total organic carbon. Using Pareto ranking, we identified HLB+Coconut as the optimal SPE method, which exhibited the highest level of water sample biotoxicity and recovered the most chemicals in water samples. We found that the biotoxicity outcomes of the extracted water samples significantly and positively correlated with the chemical extracting efficiencies of the SPE methods. Moreover, we observed synchronous changing patterns in biotoxicity outcome and chemical extracting efficiencies in response to increasing sample volumes per cartridge (SVPC) during SPE. Our findings underscore that higher chemical extracting efficiency of SPE corresponds to higher biotoxicity outcome of environmental water samples, providing a scientific basis for standardization of SPE methods for adequate assessment of biotoxicities of environmental waters. [Display omitted] [ABSTRACT FROM AUTHOR]

The high concentration of active substances in tomato extraction is correlated with its anti-tyrosinase and antioxidant effect activity. We established the optimum ultrasound extraction conditions for maximizing the yield of active substances. The four important factors (ethanol concentration, extraction time, extraction temperature, and solid-liquid ratio) that greatly affected ultrasonic extraction were selected to set up a single-factor test and investigate the effects of inhibitory activity on tyrosinase. According to the result of the single-factor test, the orthogonal experiment was conducted to select the optimum process parameter of extracting a total active substance from tomatoes by the alcohol extraction method. The factors affecting the extraction of active substances from tomatoes by an ultrasonic assistant method in order were as follows: ethanol concentration > solid-liquid ratio > extraction temperature > extraction time. The optimum process condition from the orthogonal experiment was as follows: ethanol concentration of 80%, solid-liquid ratio of 1:6, extraction temperature of 50°C, and extraction time of 50 min, under which the average anti-tyrosinase activity of active substances was 32.77% through the tyrosinase inhibition assay. [ABSTRACT FROM AUTHOR]

Parabens are frequently used preservatives in food and personal care products. These are also termed endocrine disruptors which have the potential to damage the endocrine system Therefore, an easy and facile extraction and detection of parabens are critically important. This work evaluates different magnetic sorbents such as Fe3O4@MIL‐101(Cr), Fe3O4@MIL‐101(Cr)@NH2, and Fe3O4@MIL‐101(Cr)@SO3H for magnetic solid phase extraction (MSPE) and further selected Fe3O4@MIL‐101(Cr)@NH2 to determine paraben content in chili powder and facial toner samples. Fe3O4@MIL‐101(Cr)@NH2 is an efficient sorbent material specially designed for MSPE, which profoundly extracted nine parabens within a short span of just 6 min, driven by π–π interaction and hydrogen bonding. And a detailed optimization and LC–MS/MS analysis was carried out. Fe3O4@MIL‐101(Cr)@NH2 exhibited superior extraction efficiency, enabling subsequent quantification via LC–MS/MS. The limit of detection ranged from 0.063 to 0.622 ng mL−1 and limit of quantification of 0.211 to 2.073 ng mL−1 were a good recovery in the range of 76.2%–108%. An effective detection of eight parabens in chili powder and four parabens in facial toner samples was determined indicating that Fe3O4@MIL‐101(Cr)‐NH2 sorbents are suitable for MSPE. [ABSTRACT FROM AUTHOR]

In this study, the attapulgite nanoparticle was immobilized on the surface of magnetic nanoparticle Fe3O4 via a novel surface covalent reaction method for the magnetic solid phase extraction (MSPE) for the first time. The surface covalent reaction method has the advantages of controllable steps, and can make the magnetic attapulgite nanoparticle (MANP) have good homogeneity and high stability. Field emission scanning electron microscopy, equipped with an energy dispersive spectrometer, Nitrogen adsorption BET, X-ray diffraction and Fourier transform infrared spectroscopy were applied to characterize the prepared MANP, confirming that the attapulgite nanoparticle could be effectively immobilized on the surface of magnetic nanoparticle Fe3O4 via covalent reactions. Under optimal conditions of the MSPE experiment based on the MANP, the limits of detection were found to be 10 ng/mL for melamine and 3 ng/mL for cyromazine with a relative standard deviation < 10% by a high-performance liquid chromatography system. Meanwhile, 0.1 mg/mL melamine in milk and 0.1 mg/mL cyromazine in cucumber can also be detected according to our MSPE procedure. More importantly, the MANP still has good magnetism and enrichment efficiency after several decades of use. These results showed that the MANP prepared by our method is a kind of promising material for the MSPE. [ABSTRACT FROM AUTHOR]

A novel magnetic nanomaterial with Fe3O4 as the core, PS-DVB as the shell layer, and the surface modified with C18 (C18−PS−DVB−Fe3O4) had been synthesized by seeded emulsion polymerization. C18−PS−DVB−Fe3O4 retains the advantages of the chemical stability, large porosity, and uniform morphology of organic polymers and has the magnetic properties of Fe3O4. A simple, flexible, and efficient magnetic dispersive solid phase extraction (Mag-dSPE) method for the extraction of preservatives, sweeteners, and colorants in river water was established. C18−PS−DVB−Fe3O4 was used as an adsorbent for Mag-dSPE and was coupled with high-performance liquid chromatography (HPLC) to detect 11 food additives: acesulfame, amaranth, benzoic acid, tartrazine, saccharin sodium, sorbic acid, dehydroacetic acid, sunset yellow, allura red, brilliant blue, and erythrosine. Under the optimum extraction conditions, combined with ChromCoreTMAQC18 (5 μm, 4.6 × 250 mm), 20 mmol/L ammonium acetate aqueous solution and methanol were used as mobile phases, and the detection wavelengths were 240 nm and 410 nm. The limits of detection (LODs) of 11 food additives were 0.6–3.1 μg/L with satisfactory recoveries ranging from 86.53% to 106.32%. And the material could be reused for five cycles without much sacrifice of extraction efficiency. The proposed method has been used to determine food additives in river water samples, and results demonstrate the applicability of the proposed C18−PS−DVB−Fe3O4 Mag-dSPE coupled with the HPLC method to environment monitoring analysis. [ABSTRACT FROM AUTHOR]

The advancement of traditional sample preparation techniques has brought about miniaturization systems designed to scale down conventional methods and advocate for environmentally friendly analytical approaches. Although often referred to as green analytical strategies, the effectiveness of these methods is intricately linked to the properties of the sorbent utilized. Moreover, to fully embrace implementing these methods, it is crucial to innovate and develop new sorbent or solid phases that enhance the adaptability of miniaturized techniques across various matrices and analytes. Graphene-based materials exhibit remarkable versatility and modification potential, making them ideal sorbents for miniaturized strategies due to their high surface area and functional groups. Their notable adsorption capability and alignment with green synthesis approaches, such as bio-based graphene materials, enable the use of less sorbent and the creation of biodegradable materials, enhancing their eco-friendly aspects towards green analytical practices. Therefore, this study provides an overview of different types of hybrid graphene-based materials as well as their applications in crucial miniaturized techniques, focusing on offline methodologies such as stir bar sorptive extraction (SBSE), microextraction by packed sorbent (MEPS), pipette-tip solid-phase extraction (PT-SPE), disposable pipette extraction (DPX), dispersive micro-solid-phase extraction (d-µ-SPE), and magnetic solid-phase extraction (MSPE). [ABSTRACT FROM AUTHOR]

The irrigation of soils with reclaimed contaminated wastewater or its amendment with sewage sludge contributes to the uptake of pharmaceuticals by vegetables growing in the soil. A multiresidue method has been devised to determine five pharmaceuticals and nine of their main metabolites in leafy and root vegetables. The method employs ultrasound-assisted extraction, clean-up via dispersive solid-phase extraction, and analysis through liquid chromatography–tandem mass spectrometry. Box–Behnken design was used to refine variables such as extraction solvent volume, time of extraction, number of extraction cycles, and the type and amount of d-SPE sorbent. The method achieved linearity (R2) greater than 0.994, precision (relative standard deviation) under 16% for most compounds, and detection limits ranging from 0.007 to 2.25 ng g−1 dry weight. This method was applied to a leafy vegetable (lettuce) and to a root vegetable (carrot) sourced from a local market. Parent compounds were detected at higher concentrations than their metabolites, with the exception of carbamazepine-10,11-epoxide. [ABSTRACT FROM AUTHOR]

For the first time, a highly permeable nanoporous carbon derived from melamine-based polybenzoxazine (NPC-PBZ-m) was used as the solid-phase extraction sorbent for trace analysis of atrazine (ATZ) herbicide in environmental water samples as a pre-treatment to enhance detection for high-performance liquid chromatography. Extraction performance was investigated using an agricultural field matrix-water sample. The parameters affecting the solid-phase extraction efficiency were carefully investigated. The optimisation conditions were determined as 200.0 mg of sorbent with an adsorption flow rate of 10.0 mL min−1, an elution flow rate of 1.0 mL min−1, and an elution volume of 3.0 mL. Moreover, it was not necessary to adjust the pH of the sample. Under these optimised extraction conditions, good linearity between 5.00 and 30.0 µg L−1 was achieved along with a limit of detection (LOD) of 1.25 µg L−1 and a limit of quantification (LOQ) of 3.79 µg L−1. Furthermore, the reusability of the NPC-PBZ-m column was found up to 8 cycles making it a new cost-effective material for herbicide enrichment. Finally, this developed method was successfully applied to analyse ATZ in water samples from rice fields, fish farms, and natural canal water, with 98–117% relative recoveries. These results indicate that NPC-PBZ-m with our proposed method is feasible and demonstrates its potential application as an effective adsorbent for herbicide enrichment. [ABSTRACT FROM AUTHOR]

Diamide insecticides represent a class of highly efficient compounds that have been widely employed in plant protection in recent years. The potential risk of exceeding residue limits in agricultural products should not be disregarded but the molecular structure of diamides dictates that the currently widely used QuEChERS cannot be extended to the analysis of their residues in food. The aim of this work is to develop a multi-residue method for diamides in vegetables using an alternative to traditional plant pigment removers. A modified QuEChERS based on the recently reported pigment remover Carbon S was established, and a multi-residue method for the determination of six diamide insecticides (flubendiamide, chlorantraniliprole, cyantraniliprole, tetrachlorantraniliprole, cyclaniliprole, and broflanilide) in melons and leafy vegetables using ultra-performance liquid chromatography with photodiode array detector (UPLC-PDA) was developed. The evaluation of this methodology showed the recoveries of the diamides in the vegetable matrices ranged from 80 to 107%, with intra- and inter-day relative standard deviations (RSDs) of less than 10%. The limits of quantification (LOQs) for these insecticides in vegetables were from 0.034 to 0.051 mg/kg. The modified QuEChERS employing carbon S exhibits environmental friendliness, high efficiency, and good reproducibility. The optimized methodology demonstrates accuracy, sensitivity, and reliability. Carbon S was used as a plant pigments remover, extending the application of QuEChERS to the determination of diamide residues in vegetables. [ABSTRACT FROM AUTHOR]

Buprenorphine is one of the most commonly used pain-killing drugs due to its lengthy duration of action and high potency. However, excessive usage of buprenorphine can be harmful to one's health and prolonged use might result in addiction. Additionally, an increasing number of cases have been documented involving the illegal use of buprenorphine. Therefore, a variety of effective and reliable methods for pretreatment and determination of buprenorphine and its main metabolite norbuprenorphine have been established. This review aims to update the current state of pretreatment and detection techniques for buprenorphine and norbuprenorphine from January 2010 to March 2022. Pretreatment methods include several traditional extraction methods, solid-phase extraction, QuECHERS, various micro-extraction techniques, etc. while analytical methods include LC-MS, LC coupled with other detectors, GC-MS, capillary electrophoresis, electrochemical sensors, etc. The pros and cons of various techniques were compared and summarized, and the prospects were provided. HIGHLIGHTS: Progress in pretreatment and detection methods for buprenorphine is demonstrated. Pros and cons of different pretreatment and analysis methods are compared. New materials (such as nanomaterials and magnetic materials) used in buprenorphine pretreatment are summarized. Newly emerged environmental-friendly methods are discussed. [ABSTRACT FROM AUTHOR]

A novel 3D magnetic nanocomposite material based on covalent organic polymers was successfully synthesized and utilized as an efficient sorbent for magnetic solid-phase extraction. It exhibited a regular core–shell structure, large specific surface area, superior stability, and paramagnetism. To evaluate its extraction efficiency, six flavonoids were tested, demonstrating maximum adsorption capacities ranging from 90 to 218 mg/g. Additionally, the material exhibited remarkable reusability and mechanical stability, maintaining its original state over eight cycles with consistent recovery. An analytical strategy combining magnetic solid-phase extraction with high performance liquid chromatography and tandem mass spectrometry was developed for the determination of flavonoids in orange, honey, soybean, and Dioscorea bulbifera L. samples. The low limits of detection (0.01–0.1 ng/mL) and limits of quantification (0.05–0.5 ng/mL), as well as satisfactory recovery (80.4–114.8%), were obtained. The linear range started from the limits of quantification to 500 ng/mL with R2 ≥ 0.9929. These results suggest that the prepared adsorbent possesses excellent adsorption capabilities for flavonoids, highlighting its significant potential for detecting these compounds in complex sample matrices. [ABSTRACT FROM AUTHOR]

A novel magnetic dispersive solid phase extraction (MDSPE) procedure based on the deep eutectic solvent (DES) modified magnetic graphene oxide/metal organic frameworks nanocomposites (MGO@ZIF-8@DES) was established and used for the efficient enrichment of estradiol, estrone, and diethylstilbestrol in cosmetics (toner, lotion, and cream) for the first time. Then, the three estrogens were separated and determined by UHPLC-UV analysis method. In order to study the features and morphology of the synthesized adsorbents, various techniques such as FT-IR, SEM, and VSM measurements were executed. The MGO@ZIF-8@DES nanocomposites combine the advantages of high adsorption capacity, adequate stability in aqueous solution, and convenient separation from the sample solution. To achieve high extraction recoveries, the Box-Behnken design and single factor experiment were applied in the experimental design. Under the optimum conditions, the method detection limits for three estrogens were 20–30 ng g−1. This approach showed a good correlation coefficient (r more than 0.9998) and reasonable linearity in the range 70–10000 ng g−1. The relative standard deviations for intra-day and inter-day were beneath 7.5% and 8.9%, respectively. The developed MDSPE-UHPLC-UV method was successfully used to determine three estrogens in cosmetics, and acceptable recoveries in the intervals of 83.5–95.9% were obtained. Finally, three estrogens were not detected in some cosmetic samples. In addition, the Complex GAPI tool was used to evaluate the greenness of the developed pretreatment method. The developed MDSPE-UHPLC-UV method is sensitive, accurate, rapid, and eco-friendly, which provides a promising strategy for determining hormones in different complex samples. [ABSTRACT FROM AUTHOR]

UV filters and benzotriazole UV stabilizers are considered emerging contaminants in the environment. LC–MS/MS and GC–MS methods, involving a single solid phase extraction protocol, were developed and validated to determine eight UV filters and seven UV stabilizers, respectively in wastewater from a wastewater treatment plant (WWTP) in Lüneburg, Germany. The LC–MS/MS method exhibited extraction recoveries of ≥ 71% at six different fortification levels with limits of detection (LODs) range of 0.02 ng mL−1 – 0.09 ng mL−1. Extraction recoveries of 47 to 119% at six different fortification levels were obtained for the GC–MS method with LODs range of 0.01 – 0.09 ng mL−1. Among the UV filters, the highest mean concentration was determined for octocrylene (OCR) in influent (3.49 ng mL−1) while the highest mean concentration was measured for 2-hydroxy-4-octyloxybenzophenone (UV 531) in influent (0.44 ng mL−1) among the UV stabilizers. Potential risk to aquatic organisms was assessed by the risk quotient approach. Only OCR presented a high risk to aquatic invertebrates whereas 2-ethylhexyl 4-methoxycinnamate (EHMC) and 2-ethylhexyl salicylate (EHS) posed high risks to algae. Benzotriazole UV stabilizers presented negligible risks to aquatic invertebrates and fish. This work reports the detection of rarely studied 4-aminobenzoic acid (PABA) and UV 531 in WWTP influent and effluent. The occurrence and risk assessment of target benzotriazole UV stabilizers in wastewater from a German WWTP was demonstrated for the first time. [ABSTRACT FROM AUTHOR]

The electron layer structure and physical chemical properties of rare earth elements are very similar, rare earths are difficult to separaterare. Therefore, the extraction of rare earth is always research hot issue in rare earth metallurgy. A new emulsion extractant was prepared with 6%D2EHPA as the flow carrier, 5 % Tl 54 as the surfactant, 3.0 mol/L HCl solution as the inner water phase, sulfonated kerosene as the membrane solvent and control Roi of 1.5. By using the emulsion extractor to extract La3+, Ce3+, Sm3+, Eu3+, Ho3+ and Er3+ in sulfuric acid system, the optimal kinetic conditions for the extraction of RE (III) by emulsion film method (ELM) were determined. The results show that under optimal kinetic conditions of emulsification time of 5 min, extraction time of 6 min, emulsion to water ratio (Rew) of 0.5, extraction temperature of 25 °C, the outer water phase is rare earth element aqueous solution, the highest extraction rate of La3+ is 99.92%, the maximum enrichment ratio is 3.33, and the mass transfer rate k = 9. 35 X 10-10 m/s. The ELM shows excellent extraction performance and enrichment effect for low concentration La3+ solution. [ABSTRACT FROM AUTHOR]

Glyphosate is the most used herbicide in agriculture. Its major metabolite is AMPA (aminomethylphosphonic acid), but N-acetyl-AMPA and N-acetylglyphosate are also metabolites of interest. For risk assessment, a general residue definition was proposed as the sum of glyphosate, AMPA, N-acetyl-glyphosate and N-acetyl-AMPA, expressed as glyphosate. A confirmatory method for glyphosate in fat, liver and kidneys, as well as a confirmatory method for AMPA and N-acetyl-glyphosate in all matrices, are still missing. In this paper, we present a method for the quantitative determination of glyphosate residues and its metabolites AMPA, N-acetyl-AMPA and N-acetyl-glyphosate by liquid chromatography–mass spectrometry (LC-MS/MS) in adipose tissue, liver, eggs, milk and honey without derivatization. Different chromatographic columns were tested, with the Hypercarb column providing the best results. The analytes were eluted with mobile phases of acidified water with 1.2% formic acid and 0.5% formic acid in acetonitrile. Sample purification procedures were also optimized by varying the solvent extraction mixtures (water, methanol and mixture ψ (methanol, water) = 1:1, each with the addition of 1% formic acid (v/v)), using different sorbents in solid phase extraction (SPE) (polymeric cationic (PCX) and anionic (PAX)) and using dispersive solid phase extraction (dSPE) (C18 and PSA) by modifying the extraction procedures. Finally, the analytes were extracted from the samples with 1% formic acid in water (v/v). Milk and adipose tissue were purified by the addition of dichloromethane, while liver and egg samples were purified by SPE with a mixed cation exchange sorbent and ultrafiltration with cut-off filters. The proposed analytical procedures were validated according to SANTE/11312/2021 guidelines: linearity, limits of quantification, precision and accuracy were determined for all matrices. The limits of quantification (LOQs) ranged from 0.025 to 0.2 mg kg−1. Precision, expressed as relative standard deviation, was <20%, while accuracy, expressed as analytical recovery, ranged from 70% to 120%. During method validation, the measurement uncertainty was estimated to be <50% for all analytes. Good validation parameters according to the SANTE document were achieved for all analytes. Therefore, the method can be considered reliable and sensitive enough for routine monitoring of polar pesticides. The application of the accredited method in routine analysis will provide data that are useful for the re-evaluation of risk assessment studies in foods of animal origin. [ABSTRACT FROM AUTHOR]

Emerging contaminants (ECs) are substances that have no defined environmental quality standards or regulations, and have the potential to pose major adverse impacts on the environment and human health. The detection of contaminants in the natural environment is the key step for establishing precise environmental risk assessment approach for ECs. However, ECs come from different origins with various physicochemical properties, making their detection a complicated process. Moreover, their presence in the aquatic environment at trace concentration range (ng/L-µg/L), requires an accurate detection at low concentration levels. This study aims to develop an efficient analytical method for simultaneous determination of 5 different ECs in aqueous solution based on solid phase extraction technique (SPE) followed by liquid chromatography-mass spectrometry (LC–MS/MS). High recovery rates (72% to 114%) were achieved for all targeted compounds. Ciprofloxacin (CIP), diuron (DIU), terbutryn (TER) and diclofenac (DIC) had a limit of detection (LOD) of 5 µg/L and a limit of quantification (LOQ) of 10 ng/L, while LOD and LOQ for EE2 were 25 µg/L and 50 ng/L, respectively. These results confirm that the optimized method can be applied for extraction and analysis of ECs from different classes in the aquatic environment. [ABSTRACT FROM AUTHOR]

Magnetic solid-phase extraction (MSPE) is a highly effective method for separating metal ions from aquatic solutions, making it a popular choice for metal ion separation. This study investigated the behavior of Fe3O4@SiO2-SH core–shell composites for the adsorption and recovery of silver ions. The quality of the synthesized adsorbent was verified using XRD, FT-IR, EDS, FE-SEM, and EDAX-map analyses. Magnetic properties and surface charge changes were assessed using VSM and Zeta potential analyses. By implementing the classic OFAT method, the study evaluated the effect of various parameters on silver adsorption, such as pH, composite dosage, initial Ag+ concentration, temperature, and secondary metal ions. Results showed that the proposed composite had a high maximum adsorption capacity (112 mg/g) at pH = 6, ambient temperature, 0.1 g/L adsorbent dosage, and silver concentrations greater than 25 mg/L. The composite demonstrated good selectivity in Ag+ separation from a bimetallic solution containing silver and mercury ions. The results also showed that 1M HNO3 and 1M HCl solutions released over 78% and 70% of absorbed ions from the composite surface, respectively. However, the HCl solution enabled the precipitation of almost all desorbed Ag+, providing a selective recovery of silver ions. [ABSTRACT FROM AUTHOR]

A novel, simple, fast and sensitive method for the simultaneous analysis of heavy metals such as Cd(II), Cr(III), Co(II), Pb(II) and Cu(II) in hair samples based on complexometric method with EDTA and using solid-phase extraction with graphene oxide coupled with capillary electrophoresis has been developed. Under the optimised conditions, the proposed methodology had limits of detection from 5.7 to 16.8 µg kg−1 with intra- and inter-day repeatabilities <5% (in respect to relative standard deviation) in all cases. The proposed method was successfully employed for determination of heavy metals in the analysis of 20 hair samples. All samples were positive for at least one of the heavy metals studied with concentrations of 1.2 ± 1.0 mg kg−1 Cd(II), 7.2 ± 4.0 mg kg−1 Cr(III), 0.9 ± 0.8 mg kg−1 Co(II), 0.6 ± 0.2 mg kg−1 Pb(II) and 2.5 ± 0.3 mg kg−1 Cu(II). The method is an easy, robust and efficient strategy for determination of heavy metals in complex matrices. [ABSTRACT FROM AUTHOR]

Magnetised attapulgite (ATP-Fe3O4) adsorbent was synthesised using a sonochemistry approach for the solid phase extraction of As3+ from stimulated and unrefined crude oil samples. The average size of the Fe3O4 nanoparticles estimated from the Transmission Electron Microscopy (TEM) image was 10 nm. The TEM analysis also showed that Fe3O4 nanoparticles agglomerated in the ATP's tube and on its surface. The X-ray diffraction analysis (XRD) indicates that the crystallinity of the ATP reduced after the magnetisation process. The saturation magnetisation of the ATP-Fe3O4 was determined to be only 2.8 emu g-1. Under the optimum conditions (pH = 7, adsorbent dosage = 0.6 g, contact time = 90 min and sample volume = 50 mL), the As3+ removal was more than 98% for both types of oil. The limits of detection (LOD) and relative standard deviations (RSD%) were 2.88 ng mL-1 and 0.3423%, respectively. The adsorption process follows the pseudo-first-order kinetic model (R2 = 0.9696) and adheres to the Langmuir isotherm model (R2 = 0.9925). The reusability study showed that ATP-Fe3O4 is highly stable and can be reused five times with almost 100% removal efficiency. This research outcome aligns with the United Nations Sustainable Goal 7, Affordable and Clean Energy. [ABSTRACT FROM AUTHOR]

A new modified cellulose with diaminoguanidine (Cel-Gua) synthesized for specific recovery of Cu (II), Cd (II), and Hg (II) from the alum sample. Cellulose was silanized by 3-chloropropyltrimethoxysilane and then was modified with diaminoguanidine to obtain N-donor chelating fibers. Fourier transform-infrared spectroscopy, scanning electron microscopy, X-ray diffraction, zeta potential, electrons disperse X-ray analysis, elemental analyses (C, H and N), and thermogravimetric analysis were used for characterization. Factors influencing the adsorption were thoroughly examined. Under the optimal conditions, the Cel-Gua sorbent displayed maximum adsorption capacities of 94.33, 112.10 and 95.78 mg/g for Cu (II), Cd (II), and Hg (II), respectively. The sorption process of metal ions is equipped by kinetic model PSO and Langmuir adsorption isotherm. The calculated thermodynamic variables confirmed that the adsorption of Cu (II), Cd (II) and Hg (II) by Cel-Gua sorbent is a spontaneous and exothermic process. In our study, we used the molecular operating environment software to conduct molecular docking simulations on the Cel-Gua compound. The results of the docking simulations showed that the Cel-Gua compound displayed greater potency and a stronger affinity for the Avr2 effector protein derived from Fusarium oxysporum, a fungal plant pathogen (code 5OD4). The adsorbent was stable for 7 cycles, thus allowing its safe reutilization. [ABSTRACT FROM AUTHOR]

The study aimed to analyze nusinersen metabolites in the cerebrospinal fluid samples using ion-pair reversed-phase ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. Three different sample preparation methods were tested for extraction and purification, but solid phase extraction appeared to be the most suitable, allowing a significant sample enrichment (40-fold). This step was necessary to detect and identify metabolites of nusinersen in the cerebrospinal fluid. The developed and applied analytical procedure enabled the identification of nusinersen metabolites: sequences shorter by several nucleotides from the 3′ end; shorter by several nucleotides from both the 3′ and 5′ ends; and some depurination products. To the best of our knowledge, this is the first report on the analysis and identification of nusinersen metabolites in cerebrospinal fluid samples taken from children with spinal muscular atrophy treated with Spinraza. [ABSTRACT FROM AUTHOR]

There are some notable drawbacks of ordinary magnetic effervescent tablets including their quick disintegration, hygroscopicity, and impracticability for field use. In order to solve the above problems for further extraction and preconcentration of three phenolic pesticides from crop flour samples, an effervescent tablet-assisted acidic ionic liquid-based in situ solvent formation magnetic solid-phase extraction (ETA-AIL-MSPE) technique was developed. In contrast to conventional imidazole ionic liquids, acidic ionic liquids can be employed as an acid source for effervescent processes in addition to being used as extractants. Not only does this reduce the need for organic solvents, but the production of CO2 by the effervescent tablet also provides a rapid dispersion effect, removing the requirement for further dispersion stages and streamlining the experiment. The magnetic effervescent tablet is made of Na2CO3 as an alkaline source, [BMIM][HSO4] as extractant and acidic sources, NaCl as a viscosity modifier, and Fe3O4 as magnetic nanoparticles. The Plackett–Burman design and the central composite design were used to screen and optimize three key variables (93 mg of Na2CO3, 451 mg of AIL, and 37 mg of Fe3O4), respectively. Through the integration of high-performance liquid chromatography-diode array detection (HPLC-DAD), the ETA-AIL-MSPE technique provided enhanced recoveries of 85.0–107.2% and limits of detection of 0.14–0.17 μg kg−1 for three representative species (ioxynil, bromoxynil, and dinoseb) in four different types of crop flour samples. For both intra-day and inter-day precision, the relative standard deviations were below 7.7%. Generally, the recently developed technique is convenient, efficient and environmental-friendly, and it has great potential for on-site sample preparation for the detection of phenolic pesticides in crop flour samples. [ABSTRACT FROM AUTHOR]

In this work, we test metal–organic frameworks (MOFs) as sorbents in the solid-phase extraction (SPE) technique to determine chemical warfare agents (CWAs) and their related compounds in water samples. During this study, we used 13 target compounds to test the selectivity of MOFs thoroughly. Three MOFs were used: MIL-100(Fe), ZIF-8(Zn), and UiO-66(Zr). The obtained materials were characterized using FT-IR/ATR, SEM, and XRD. CWA's and related compounds were analyzed using gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). The effect of the type of elution solvent and the amount of sorbent (MOFs) in the column on the efficiency of the conducted extraction were verified. The LOD ranged from 0.04 to 7.54 ng mL−1, and the linearity range for the analytes tested extended from 0.11/22.62 (depending on the compound) to 1000 ng mL−1. It was found that MOFs showed the most excellent selectivity to compounds having aromatic rings in their structure or a "spread" spatial structure. The best recoveries were obtained for DPAA, CAP, and malathion. Environmental water samples collected from the Baltic Sea were analyzed using an optimized procedure to verify the developed method's usefulness. [ABSTRACT FROM AUTHOR]

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Copyright of Shipin Kexue/ Food Science is the property of Food Science Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)