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A new nanocomposite based on alginate microbeads impregnated with novel strontium–aluminum layered double hydroxide (Sr‐Al LDH) incorporated with choline chloride‐urea deep eutectic solvent (ChCl‐U DES) was introduced. The microbeads and LDH were characterized by adsorption/desorption isotherms, Fourier‐transform infrared spectroscopy, SEM, and x‐ray diffraction. The adsorbent was employed for determining penicillin G (PENG) using dispersive solid‐phase extraction prior to HPLC analysis. The extraction efficiency of the adsorbent, compared with that of unmodified alginate, showed a 2.5‐fold increase. Significant parameters, including elution conditions, sorbent composition and mass, adsorption time, and sample pH, were optimized. The LOD was 0.4 µg kg−1, and the linear range was 1.4–500 µg kg−1. The LOQ (1.4 µg kg−1) was lower than the established maximum level for PENG by the European Union (4 µg kg−1). Enrichment factor and synthesis reproducibility were also investigated. The method's accuracy was evaluated through PENG analysis in dairy products and water, with recoveries of 81%–107% (RSDs < 7.6%). The procedure's greenness was assessed using the Analytical Eco‐scale and achieved excellent green credentials. To the best of our knowledge, this is the first report on the synthesis and application of a novel alginate composite for the extraction of PENG from dairy and water samples. [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]

As a widely occurring natural product, alkaloids have garnered increasing attention in drug research and development. The efficient, convenient, and environmentally friendly separation and detection of alkaloid compounds from diverse natural products has garnered increasing attention in recent research. Molecular imprinting technology (MIT) is recognized as an effective method for the selective extraction and separation of alkaloids from complex samples due to its capacity for specific recognition. To date, no comprehensive review has been published on the separation and purification of alkaloids using MIT, particularly regarding the sustainability aspects of this technology. In this paper, we review the general preparation methods of molecularly imprinted polymers (MIPs) for alkaloids, including bulk polymerization, precipitation polymerization, magnetic polymerization, and emulsion polymerization. Additionally, we summarize various applications of MIPs for alkaloids, such as different forms of MIP‐based solid phase extraction (MISPE) and MIP‐based sensors for alkaloids detection. Finally, we address some unresolved issues and anticipate future developments in the field. [ABSTRACT FROM AUTHOR]

Huperzine A is a reversible and selective cholinesterase inhibitor and has been approved for the treatment of Alzheimer's diseases. In this study, we developed a highly sensitive and specific ulta‐high‐performance liquid chromatography–tandem mass spectrometry method for the determination of Huperzine A in rat plasma. An aliquot of 50 μL of rat plasma sample was pretreated with 200 μL of acetonitrile‐methanol (v/v; 1:1) containing 0.2% formic acid followed by solid phase extraction. The resulting sample was separated on a Waters ACQUITY BEH C18 column using acetonitrile and water containing 0.2% formic acid as mobile phase, at a flow rate of 0.3 mL/min. Multiple‐reaction monitoring (MRM) mode was used for quantitative analysis of Huperzine A in positive electrospray ionization. In the concentration range of 0.01–10 ng/mL, Huperzine A showed excellent linearity with correlation coefficient > 0.998. The intra‐ and inter‐day RSD% were less than 9.7%, while the RE% ranged from −6.7% to 10.0%. The mean recovery was >84.5%. The validated method was demonstrated to be selective, sensitive, and reliable, which has been successfully applied to pharmacokinetic study of Huperzine A in rat plasma. Huperzine A displayed a long half‐life in rat plasma and high oral bioavailability. [ABSTRACT FROM AUTHOR]

Rationale: High‐resolution mass spectrometry (HRMS) combined with electrospray ionization (ESI) has been the most useful technique for molecular characterization of dissolved organic matter (DOM) derived from diverse sources. However, the comprehensive detection of DOM composition was hindered by ionization suppression observed in ESI sources. HRMS coupled with liquid chromatography (LC) is a potential tool for comprehensive molecular characterization of DOM. Methods: The Suwannee River fulvic acids (SRFAs) and two DOM samples from seawater and refinery wastewater extracted by solid phase extraction (SPE) were analyzed by LC‐Orbitrap MS coupled with ESI. The mobile phases, solvent composition, and gradient in the LC‐Orbitrap MS analysis were optimized. Results: The number of detected molecular formulae of SRFAs by online LC‐Orbitrap MS was significantly increased by approximately 40% compared to direct injection. These additional detected compounds are mainly protein and lignin‐like compounds, with a low O/C ratio and high H/C ratio. For the SRFAs, the relative standard deviations (%) of reproducibility are 5.51, 2.33, 7.97, and 1.80 for average O/C, H/C, double bond equivalent, and modified aromaticity index, respectively. Conclusions: This study proposed a simple and rapid method based on LC‐Orbitrap MS for an in‐depth analysis of the molecular composition of DOM, achieving a remarkable analysis time of only 5 min per sample. The rapid method provides a dependable and efficient approach for the molecular characterization of DOM, thereby advancing our comprehension and investigation of DOM across diverse ecosystems. [ABSTRACT FROM AUTHOR]

Synthetic cocaine analogs are designer drugs that recently emerged as non‐controlled substitutes for their parent drug. Among them, nitracaine is of particular concern for its psychoactive effect. In this work, we present a thorough characterization of the electrochemical behavior of nitracaine, with a final quantification performed by differential pulse voltammetry (DPV) in ethanol/lithium perchlorate 0.1 M. The selectivity of the method and reproducibility of results were assessed. LOQ of 0.3 μg mL−1 and a linear dynamic range of up to 400 μg mL−1 were obtained. In addition, recoveries from 85 % to 101 % were achieved on both simulated and real samples. For nitracaine analysis in urine, a clean‐up and a preconcentration step by solid phase extraction (SPE) using the adsorbent Florisil have been developed and optimized through the Design of Experiments (DoE) strategy, thus achieving an enrichment factor of 20. [ABSTRACT FROM AUTHOR]

A sensitive analytical procedure for simultaneous extraction and determination of bisphenol A and alkyl phenols, namely, 4‐sec‐butylphenol, 4‐tert‐butylphenol, and 4‐tert‐amylphenol from aqueous samples with metal–organic framework (MOF)‐based dispersive micro‐solid‐phase extraction (D‐µSPE) and high‐performance liquid chromatography (HPLC) technique is developed. Sample contaminants were preconcentrated with amino‐functionalized aluminum MOF and later eluted with acetonitrile. The reconstituted sample was subjected to HPLC analysis. Various procedural parameters related to D‐µSPE were optimized. Under optimized preconcentration and chromatographic conditions, calibration curves with excellent linearity (R2 > 0.9986) in the working range of 0.25–100 ng mL−1 were prepared. Limit of detection (S/N = 3) for every analyte within the range of 0.020–0.022 ng mL−1 was obtained. Analyte's recovery 91.16%–97.01% (RSD = 1.02–3.01) for intraday and 89.86%–95.83% (RSD = 1.15–3.13) for inter‐day analysis was obtained from real water samples. [ABSTRACT FROM AUTHOR]

Abnormal levels of catecholamine (CA) neurotransmitters and their metabolites in biological fluids can lead to various neurological disorders. Herein, a boric acid‐functionalized hypercrosslinked polymer was prepared and utilized as a sorbent for the dispersive solid‐phase extraction of CAs and their metabolites in rat serum. By combination with a high‐performance liquid chromatography‐fluorescence detector, the extraction parameters for the seven target analytes were optimized. Under the optimal extraction condition, the methodology for the quantitative analysis of CAs and their metabolites in rat serum samples was established. The limits of detection and limits of quantification were found to be in the ranges of 0.010–0.015 and 0.033–0.050 ng/mL, respectively. The results demonstrated satisfactory recoveries, with values ranging from 88.02% to 113.27%, accompanied by relative standard deviations within the range of 2.69%–9.59%. In addition, the method showed good anti‐interference ability (matrix effect ranged from 2.64% to 18.07%). The developed method was validated for the determination of CAs and their metabolites in normal and Alzheimer's disease model rats' serum, which proved the promising application of the method for CAs neurotransmitter analysis in biological samples. [ABSTRACT FROM AUTHOR]

This work introduces a novel method of recovering bioactive berry natural products (BNPs) using solid phase extraction with metal‐organic frameworks (MOF‐SPE). Two pyrene‐based MOFs with different structural topologies, Al‐PyrMOF and Zr‐NU‐1000, were evaluated for their ability to capture and desorb BNPs, including ellagic acid, quercetin, gallic acid, and p‐coumaric acid. Time‐dependent BNP uptake via dispersive SPE revealed that NU‐1000 outperformed Al‐PyrMOF in capturing all BNPs. Our findings show NU‐1000 demonstrated a higher and more consistent BNP capture profile, achieving over 90 % capture of all BNPs within 36 h, with only a 9 % variation between the most and least effectively captured BNPs. In contrast, Al‐PyrMOF, displayed a staggered uptake profile, with a significant 53 % difference in capture efficiency between the most and least effectively captured BNP. However, when a BNP mixture was used at a loading concentration of 50 μg/mL, Al‐PyrMOF outperformed NU‐1000, capturing over 70 % of all BNPs. Al‐PyrMOF also exhibited improved BNP recovery, with a minimum of two‐fold greater amount recovered for all BNPs. Further testing with a BNP mixture at a concentration of 15 μg/mL demonstrated that Al‐PyrMOF efficiently concentrated all BNPs, achieving a maximum extraction factor of 2.71 observed for quercetin. These findings highlight the use of Al‐PyrMOF as a MOF‐SPE sorbent for recovering bioactive BNPs. [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]

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]

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]

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]

Amphetamines (AMPHs) and their derivatives are potent central nervous system stimulants, in 2020 an astonishing 34 million regular users were reported worldwide. Consequently, there has been a critical need for the development of methods capable of detecting these compounds in alternative biological matrices. The review article discusses the analysis of amphetamines and their derivatives in alternative biological matrices, such as hair and oral fluid (OF), using liquid chromatography‐mass spectrometry. Compiles data from 28 articles published between 2012 and 2022, focusing on 13 articles on OFs and 15 on hair analysis. The article highlights the advantages of using these alternative matrices, including less invasive collection methods, greater sample stability, and simplified extraction processes. Additionally, prevalent analytical practices such as the use of C18 columns and the incorporation of formic acid and methanol into mobile phases are discussed. Furthermore, it demonstrates that the most used method for collecting OF is the Quantisal device, as well as solid phase extraction is also the most used for the same matrix. The review serves as a guide for researchers interested in analytical methods for identifying AMPHs, offering insights into advances, challenges, and the most used in the area. [ABSTRACT FROM AUTHOR]

The analysis of UV filters (UVFs) in water has become increasingly important due to their adverse effects on aquatic organisms and humans. This study describes a method for the determination of benzophenone derivatives UVF in wastewater samples. The selected UVFs are 2‐hydroxy‐4‐methoxybenzophenone (BP‐3), 2,4‐dihydroxybenzophenone (BP‐1), 4‐hydroxybenzophenone (4HB), 2,2′‐dihydroxy‐4‐methoxybenzophenone (DHMB) and lastly, 4,4′‐dihydroxybenzophenone (4DHB). The method includes solid‐phase extraction (SPE) of analytes from wastewater followed by on‐line derivatization with bis(trimethylsilyl)trifluoroacetamide (BSTFA) and analysis with GC‐MS/MS. Method validation studies resulted in good recoveries (86–112%), relative standard deviation RSD = 0.8 and 7.3%, the limits of detection LODs = 1.00–10.8 ng/L, and the limits of quantification LOQs = 3.00–32.3 ng/L. The method was successfully applied to domestic wastewater samples collected from influent and effluent of touristic hotels' biological wastewater treatment plants. BP‐3 (24–1765 ng/L), BP‐1 (8–703 ng/L), 4HB (26–96 ng/L), and 4DHB (20–22 ng/L) were the common benzophenone derivatives in the influent wastewater while effluent contained mainly BP‐1 (8–32 ng/L), 4HB (12–57 ng/L) and 4DHB (20–102 ng/L). These results indicate that BP‐3 and BP‐1 are biodegraded in the treatment processes. However, 4HB and 4DHB are resistant to degradation and they are the main benzophenone metabolites discharged to receiving media. [ABSTRACT FROM AUTHOR]

Copper ions in wastewater present substantial environmental hazards, toxic to aquatic species and prone to bioaccumulation. Addressing this, we present a novel cross‐linked polythiourethane (C‐PTU) as a promising chelating adsorbent for the effective removal of copper ions from wastewater. A new monomer, 5‐(2,2,2‐trifluoroacetamide) benzene‐1,3‐bis(carbonyl) isothiocyanate (TFA‐ITC), was synthesized and further condensed with a 1,4‐butane diol to produce a trifluoroacetamide functionalized polythiourethane (TFA‐PTU) and subsequently generating amine functionalized polythiourethane (A‐PTU). The cross‐linking reaction was carried out through amino groups present on the polymer backbone with terephthaloyl chloride, resulting in the formation of C‐PTU. The monomer and polymers underwent characterization using Fourier transform infrared, 1H, and 13C nuclear magnetic resonance spectroscopy, with X‐ray diffraction analyzing the resin's chain alignment. Thermogravimetric and differential scanning calorimetry assessed C‐PTU's thermal properties. The adsorption process for Cu(II) ions was studied using atomic absorption spectroscopy, optimizing conditions for maximal uptake. Results revealed that C‐PTU exhibited a significant adsorption capacity for Cu(II) ions, reaching 67% after a 2 h contact time, with optimal adsorption occurring at pH 6. The Langmuir adsorption isotherm described the sorption mechanism, indicating favorable monolayer cation adsorption via coordination with donor sites on C‐PTU. This research presents a viable solution for copper ion contamination in wastewater, illustrating C‐PTU as an efficient, environmentally friendly adsorbent, marking progress toward cleaner water resources. [ABSTRACT FROM AUTHOR]

We developed a simple, paper‐based device that enables sensitive detection by mass spectrometry (MS) without solid phase extraction or other sample preparation. Using glass fiber filter papers within a 3D printed holder, the device employs electrokinetic manipulations to stack, separate, and desalt charged molecules on paper prior to spray into the MS. Due to counter‐balanced electroosmotic flow and electrophoresis, charged analytes stack on the paper and desalting occurs in minutes. One end of the paper strip was cut into a sharp point and positioned near the inlet of a MS. The stacked analyte bands move toward the paper tip with the EOF where they are ionized by paper spray. The device was applied to analysis of PFAS in tap water with sub part‐per‐trillion detection limits in less than ten minutes with no sample pretreatment. Analysis of opioids in urine also occurs in minutes. The crucial parameters to enable stacking, separation, and MS ionization of both positively and negatively charged analytes were determined and optimized. Experimental and computational modeling studies confirm the electrokinetic stacking and analyte transport mechanisms. On‐paper separations were carried out by stacking analyte bands at different locations depending on their electrophoretic mobility, achieving baseline separation in some cases. [ABSTRACT FROM AUTHOR]

Short‐chain fatty acids (SCFAs) are organic acids with carbon atoms less than six, released through fermentation products by intestinal microbiome, having multiple physiological activities. Considering weak acidity and high volatility, derivatization or liquid–liquid extraction is essential, which is time consuming. Headspace‐solid‐phase dynamic extraction (HS‐SPDE) coupled with gas chromatography‐mass spectrometry is automated and effortless to determine SCFAs in rat feces. The extraction procedure is performed by aspirating and discharging the headspace cyclically through a steel needle, coated with an inner polyethylene glycol sorbent. The key parameters of SPDE were optimized including coating type, incubation time and temperature, and number of extraction strokes. Besides, salting‐out was conducted. Then, a method by HS‐SPDE‐GC‐MS was established and validated. It only took 3‐min incubation time, 4.5 min extraction time, and 13 min chromatographic separation in a run. The recovery, linearity, limit of quantification, and stability were evaluated. Then, the proposed method was applied to analyze rat feces including 18 rats with liver injury and 23 normal controls. Mann–Whitney U test indicated that the concentrations of six SCFAs in normal rat feces were higher than those with liver injury. This method provides a choice for fast, solvent‐free, automated, and high‐throughput analysis of SCFAs. [ABSTRACT FROM AUTHOR]

Sample preparation, including extraction, separation, and purification, is a vital process for natural product analysis. As an attractive sample pretreatment method, magnetic solid‐phase extraction (MSPE) has gained plenty of attention, mainly due to its simpler operation, less consumption of organic solvents, and shorter processing time than traditional SPE. This updated review is devoted to summarizing the applications of MSPE based on different magnetic nanomaterials in the analysis of various natural products in complex matrixes, such as biological samples, plants, and Chinese herbal preparations in the past four years (2020–2023). The preparation and fabrication of different materials are briefly introduced. Furthermore, the extraction mechanism and interaction forces between adsorbent and analytes are elaborated, and the advantages and disadvantages of different adsorbents coupled with various analytical methods for MSPE of different natural products are summarized. Moreover, the future trends and opportunities for MSPE in the natural product analysis are discussed. It is expected that this work can provide updated information for future research on the applications of MSPE in such fields. [ABSTRACT FROM AUTHOR]

An amide‐based covalent organic framework (COF) was successfully synthesized using the reaction between 1,3,5‐trimesoyl chloride and ethylenediamine. The structure and morphology of the COF were characterized using Fourier‐transform infrared spectra, nuclear magnetic resonance spectroscopy, X‐ray diffraction, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, and Brunauer‐Emmett‐Teller surface area analysis. The COF was employed as a solid‐phase extraction adsorbent for the sampling and preconcentration of chlorophenols from industrial wastewater samples prior to high‐performance liquid chromatography with ultraviolet detection. The experimental parameters influencing the extraction efficiency including type and volume of eluent solvent, sample solution volume, salt concentration, sample flow rate, and sample solution pH were investigated and optimized using a response surface methodology employing Box‐Behnken‐design. Under optimized conditions, calibration curves exhibited good linearities over the range of 0.003–10 µg/mL with determination coefficients (R2) ranging from 0.9982 to 0.9999. The method's limits of detection ranged from 0.001 to 0.01 µg/mL. Good repeatability was achieved with relative standard deviations below 4.7%. The developed procedure utilizing the COF adsorbent was successfully applied to determine chlorophenols accurately and precisely in various industrial wastewater samples. [ABSTRACT FROM AUTHOR]

In this work, core‐shell material with a special structure was designed and applied in solid‐phase extraction (SPE) for non‐steroidal anti‐inflammatory drugs (NSAIDs) combined with high‐performance liquid chromatography. Based on the advantages of core‐shell ZIF‐8@ZIF‐67 (Zeolite imidazole ester framework materials [ZIFs]), effective derivatization treatment was carried out to partially vulcanize the original ZIFs, resulting in a special and new double‐core‐shell structural material CoS/ZIF‐67/ZnS/ZIF‐8 (ZIFs@ZnS@CoS) with porous surface and center hollow. The multiple forces caused by the rich chemical structure, the large specific surface area caused by the special pore structure, and the effective protection of the ZIFs core by sulfide shell make the designed material have higher extraction efficiency and longer service life, compared with ZIF‐8@ZIF‐67 and ZIF‐8. At the same time, the established analytical method for non‐steroidal drugs had a high recovery rate (98.93%–102.10%), low detection limit (0.11–0.27 µg/L), and wide linear range (1–200 µg/L) within a good correlation coefficient R2 (0.9978–0.9993). Satisfactory results were also obtained from the extraction of NSAIDs from the Yellow River water samples. These results indicate that the designed double‐core‐shell structure material can effectively exert its structural advantages and become a promising extraction material. [ABSTRACT FROM AUTHOR]

A fast and effective analytical method with biomass solid‐phase microextraction sorbent combined with a high‐performance liquid chromatography‐ultraviolet detector was proposed for the determination of benzoylurea (BU) insecticides in tea products. The novel sorbent was prepared by activating and then carbonizing water hyacinth with a fast growth rate and low application value as raw material and showed a high specific surface area and multiple interactions with analytes, such as electrostatic action, hydrogen bonding, and π‐π conjugation. After optimizing the three most important extraction parameters (pH [X1], sample loading rate [X2], and solution volume [X3]) by Box‐Behnken design, the as‐established analytical method showed good extraction performance: excellent recovery (80.13%–106.66%) and wide linear range (1–400 µg/L) with a determination coefficient of 0.9992–0.9999, a low limit of detection of 0.02–0.1 µg/L and the satisfactory practical application results in tea products. All these indicate that the water hyacinth‐derived material has the potential as a solid‐phase extraction sorbent for the detection and removal of BU insecticides from tea products, and at the same time, it can also achieve the effect of rational use of biological resources, maintaining ecological balance, turning waste into treasure, and achieving industrial production. [ABSTRACT FROM AUTHOR]

Herein, poly(aniline‐co‐pyrrole) has been synthetized and investigated to adsorb phenylbutazone (PBZ), ceftiofur (CEF) and prednisolone (PRD) in aqueous medium as proof of concept. After proper adsorbent characterization, some studies were carried out in batch process, i. e., contact time, pH, and concentration. The adsorption mechanism has been conducted using kinetic and isothermal models. It was found that the reaction equilibrium was reached in 20 min for all analytes. The best fit for the experimental data were obtained employing the models of dual‐site Langmuir–Freundlich, Fritz–Schlunder and Langmuir, with R2=0.999, 0.952 and 0.974, for PBZ, CEF and PRD, respectively. For PBZ, CEF and PRD, poly(aniline‐co‐pyrrole) provided a Qmax=238.8 mg g−1 and Kmax=0.086 L g−1, Q=0.028 mg g−1 and Kmax=3.258 L g−1, Q=13.66 mg g−1 and KL=0.005 L g−1, respectively. Finally, the copolymer was evaluated in solid phase extraction, which showed recovery around 70 % for PBZ, offering also exciting opportunities for further application in the separation process. [ABSTRACT FROM AUTHOR]

Dissolved organic carbon (DOC) in the global oceans is an important long‐term carbon sink. Connections between molecular size, reactivity, and isotopic characteristics show that DOC exists on a continuum from biologically reactive to recalcitrant. The driving mechanisms behind the creation and persistence of recalcitrant DOC remain unknown. We show mean recalcitrant DOC (isolated via solid‐phase extraction; SPE‐DOC) δ13C values are 1.3 ± 0.6‰ lower than mean total DOC δ13C between depth ranges 0–200 m and 2–4 km on three GO‐SHIP Repeat Hydrography cruises. Lowest observed δ13C values correlate with low ∆14C and proximity to deep ocean hydrothermal systems. These data support the hypothesis that reworking of DOC through the microbial carbon pump is a key driver of the ocean's long‐term carbon sink. Mass‐balance modeling shows deep‐ocean DOC not captured by SPE is enriched in 13C, highlighting the need for continued research on non‐retained DOC to predict mechanisms that drive ocean carbon storage. Plain Language Summary: The global oceans play an important role in Earth's climate, and dissolved organic carbon (DOC) (produced by surface ocean photosynthesis) has been recognized as a potential long‐term carbon sink in the deep ocean. However, the mechanisms behind the long‐term sink remain unknown. Recent research has shown that a phenomenon called the microbial carbon pump (MCP) may be a driving force in the production of long‐lasting "recalcitrant" DOC via heterotrophic consumption of nitrogen and phosphorus rich biomolecules and subsequent production of recalcitrant DOC as by‐product. The work presented here shows that this phenomenon, previously recognized on regional scales, may be systematic across the global oceans, indicated by our measurements in the Pacific, Indian, and Southern Oceans. Key Points: Solid‐phase extracted dissolved organic carbon has low isotope signatures relative to bulk dissolved organic carbon in three ocean basinsThis research supports the hypothesis that bacteria drive the storage of recalcitrant organic matter through successive reworkingIsotope measurements show hydrothermal vent influence likely captured in deep‐ocean solid‐phase extracted dissolved organic carbon [ABSTRACT FROM AUTHOR]

Batocera horsfieldi (Hope) (Coleoptera: Cerambycidae) is an important pole borer pest. It causes serious harm to various hosts, particularly Juglans regia L. (Juglandaceae). In this study, headspace solid‐phase microextraction (HS‐SPME), gas chromatography–mass spectrometry (GC–MS), and electroantennogram (EAG) responses were combined to examine the mechanism by which B. horsfieldi adults locate their host, J. regia. The results showed that J. regia contained 65 volatile compounds in all, with 36 and 42 volatile substances in bark and leaves, respectively. Moreover, terpenes accounted for the largest relative content among the volatile compounds of bark and leaves, 43.4 and 78.9%, respectively. Ten of 19 selected volatile components elicited significant EAG responses in adult B. horsfieldi, which indicated that the pest may prefer certain volatile compounds when selecting a host. Sex and volatile concentration affected the responses of B. horsfieldi. Male adults had the strongest EAG responses to 1‐octen‐3‐ol, whereas female adults had the strongest EAG responses to linalool. Host selection in B. horsfieldi was somewhat positively associated with the concentrations of the effective volatile compounds in the host. Furthermore, B. horsfieldi showed varying preferences for isomers. This work provided data support for the development of insect attractants, and laid a theoretical foundation for the ecological protection of local forestry. [ABSTRACT FROM AUTHOR]

This study introduces a new in‐syringe homogeneous liquid‐phase microextraction method for the rapid on‐site extraction of chloroanilines from water samples. Extraction was performed using a plastic syringe, eliminating the use of any electrical power source. Di‐(2‐ethylhexyl) phosphoric acid (DEHPA) served as the extractant. The process initially involved dissolving DEHPA in an alkaline solution to obtain a homogeneous solution. Subsequently, the sodium salt of DEHPA was precipitated by salting‐out, and the resulting heterogeneous mixture was filtered using a syringe filter. The precipitate containing the analytes was then dissolved in methanol for analysis by high‐performance liquid chromatography. Under optimal conditions, extraction recovery for chloroanilines ranged from 26% to 71%. Method linearity was evaluated within a concentration range of 1.0–100 µg/L, resulting in coefficients of determination exceeding 0.9987 for all analytes. Method detection limits ranged from 0.28 to 0.41 µg/L. Intra and inter‐day precision values were below 9.5% and 10.8%, respectively. The developed method was applied to determine chloroanilines in real waters, yielding acceptable recoveries ranging from 80% to 109% for spiked tap, rain, and stream waters. Additionally, the method was successfully employed for on‐site extraction of target contaminants, demonstrating no statistically significant differences compared to laboratory results. [ABSTRACT FROM AUTHOR]

Deep eutectic solvents (DESs), as a new type of eco‐friendly solvent, have attracted increasing attention on the extraction and separation of flavonoid compounds from various samples, owing to their excellent properties such as biodegradability and ease of handling with very low toxicity. This article provides a status review of the applications of DESs in the extraction of flavonoids, including the introduction of flavonoid compounds, the properties and superiority of DESs, and extraction methods (ultrasonic‐assisted extraction, heating reflux extraction, matrix solid‐phase dispersion, and solid‐phase extraction). Finally, prospects and challenges in the application of DESs on extraction and separation are extensively elucidated and critically reviewed. [ABSTRACT FROM AUTHOR]

Vacuum‐assisted headspace solid‐phase microextraction (Vac‐HS‐SPME) is a technique used to enhance SPME sampling of semi‐volatile organic compounds. Here, it was combined with a high‐capacity SPME Arrow, which features a larger volume of extraction phase and a more rugged configuration than traditional extraction fibers. An in‐depth assessment of the critical parameters was conducted to achieve optimal extraction of representative compounds from a model solid sample matrix (Ottawa sand). Operational fundamentals investigated included the types of seals needed to create a leak‐free environment under vacuum conditions; the magnitude of the vacuum applied and time needed to activate the Vac kinetics; order of sample vial preparation methods (VPMs); and other standard variables associated with extract analysis by gas chromatography‐mass spectrometry. When exploring the limits of sample VPMs, results indicated an ideal workflow requires the solid sample to be spiked before sealing the vial, allow the sample to rest overnight, then apply vacuum at a pressure of ‐677 mbar (out of ‐789 mbar maximum possible vacuum with pump and compressor used), exerted on the vial for 90 s. This work provides the necessary workflow for the optimization of Vac‐HS‐SPME sampling of analytes from solid matrices. [ABSTRACT FROM AUTHOR]

Summary: On‐site sample preparation has the advantage of combining sampling and sample preparation into a single step, thereby minimising sources of error, and eliminating the risk of analyte instability. Bubble‐driven solid‐phase microextraction (BD‐SPME) was first proposed as an on‐site pretreatment method. Oyster sauce underwent on‐site pretreatment to measure potassium sorbate levels via high‐performance liquid chromatography with a diode array detector (HPLC‐DAD), obviating the need for stirrers. The high sensitivity of the HPLC determination of potassium sorbate was obtained using BD‐SPME pretreatment with a limit of detection (LOD) of 0.03 mg L−1 and a limit of quantification (LOQ) of 0.10 mg L−1. The refined technique displayed remarkable linearity from 0.10 to 30.00 mg L−1, boasting a coefficient of determination R2 ≥ 0.998. In addition, the recoveries of potassium sorbate in oyster sauce using the method were in the range of 90.8–101.4%. Evidently, BD‐SPME in combination with HPLC‐DAD is a sensitive and promising analysis for on‐site pretreatment. [ABSTRACT FROM AUTHOR]

BACKGROUND: Biogenic amines (BAs) in high concentrations are toxic and may cause a series of health symptoms. A sensitive measurement of BA levels is essential for human health. Capillary electrophoresis (CE) has emerged for the separation of eight BAs due to simple sample preparation and highly efficient separation. However, an important drawback for CE is low sensitivity. Magnetic solid‐phase extraction (MSPE) has become a technique of interest owing to its brief operation and low solvent consumption. Hence, MSPE as a pretreatment has great potential to improve CE sensitivity for the analysis of BAs in complex food. RESULTS: Results showed that the Pt‐Co‐MWCNTs‐COOH possessed strong magnetism, good reusability, and high adsorptive ability toward eight biogenic amines based on the hydrogen bonding between the −COOH of Pt‐Co‐MWCNTs‐COOH and −NH2 groups of BAs. Using it as an adsorbent, a magnetic solid‐phase extraction coupled with capillary electrophoresis (MSPE‐CE) method was developed to effectively extract and sensitively analyze eight BAs. Under optimal conditions, the MSPE‐CE method has wide linearities (10.0–1000.0 μg L−1) and low limits of detection (1.0–6.1 μg L−1). The accuracy of the developed method yielded recovery values from 82.07% to 102.58%. Meanwhile, the BAs contents in two samples were analyzed using the MSPE‐CE method, with the results consistent with those detected by a high‐performance liquid chromatography method. CONCLUSION: Given those advantages, the established MSPE‐CE method promises the practical guidance of monitoring a variety of BAs and provides a foundation for the detection of other food hazards. © 2023 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

Mushrooms are rich in ergosterol and ergosta‐5,7‐dienol, which can be partly converted into vitamin D2 and D4 through ultraviolet (UV) light exposure. Typically, mushrooms have very low vitamin D contents, but it can be increased by UV irradiation. This process generates additional photoisomers scarcely studied in mushrooms due to analytical challenges. Here, we developed a new solid phase extraction (SPE) method to separate vitamin D2, vitamin D4, and other tri‐ and pentacyclic photoisomers from the much higher abundant ergosterol. Subsequent GC/MS analysis enabled the detection of ten photoisomers in eight UV‐treated mushroom species, including vitamin D2 (previtamin D2, tachysterol2, two suprasterol2 and trans‐vitamin D2 isomers) and vitamin D4 (previtamin D4). Quantitated vitamin D2 contents of 10–540 µg/100 g dry weight agreed well with the sparse literature data available for the investigated mushroom species. In addition, previtamin D2 (nd–1950 µg/100 g dry weight) and vitamin D4 (10–140 µg/100 g dw) were quantified in the samples. The content and photoproduct compositions varied considerably between different mushroom species. Practical applications: The novel SPE method can be applied to study the vitamin D and photoisomer content of mushrooms. [ABSTRACT FROM AUTHOR]

Steroid hormones (SHs) have received widespread attention in recent years. However, current studies of SHs have primarily focused on estrogenic substances, with androgen‐related studies being quite limited. We optimized the solid‐phase extraction (SPE) pretreatment method, as well as the enzymolysis conditions of five androgens (androstenedione, boldenone, methandienone, nandrolone, and testosterone), to simultaneously determine their concentrations in the effluent from wastewater treatment plants and surface water samples. Then we evaluated the ecological risks of the five androgens in the effluent and Pearl River basin of Guangzhou (PR China) using the risk quotient method. The recovery rates of the targets were 90% to 99% in water samples when digested with β‐glucosidase for 90 min before solid‐phase extraction, extracted with a Poly‐Sery HLB column, and washed with 15% methanol aqueous solution and 2% ammonia. The established instrument's limit of detection was between 0.02 and 0.39 μg/L, and the limit of quantification was between 0.05 and 1.29 μg/L. Androstenedione, boldenone, methandienone, nandrolone, and testosterone were detected in all samples from the 2018 and 2022 wastewater influent and the 2018 surface water, with concentrations of 3.06 × 101 ng/L to 1.33 × 103 ng/L, 1.03–8.15 × 102 ng/L, and 0.93 × 101 ng/L to 5.50 × 102 ng/L, respectively. The ecological risks of androgens in wastewater influent and surface water were medium to high and low to medium, respectively. Moreover, the biotoxicity of androgens was predicted by the Ecological Structure Activity Relationships model, with methandienone and androstenedione having the highest and lowest acute and chronic toxicities, respectively. These results suggest that the risk of environmental androgens should not be ignored and that further research should be carried out. Environ Toxicol Chem 2024;43:915–925. © 2023 SETAC [ABSTRACT FROM AUTHOR]

Aim: Currently, no information regarding the sennosides A and B content is provided on bofutsushosan extract products for ethical use. In this study, sennosides A and B in bofutsushosan extract products from eight different pharmaceutical companies and those in bofutsushosan decoction were quantitatively analyzed. Additionally, since it has been reported that sennoside A is unstable to heat, the relationship between the different decoction times of Rhubarb and the total extracted amounts of sennosides A and B was investigated. Finally, nuclear magnetic resonance (NMR)‐based metabolomics analysis was performed on Rhubarb extracts to evaluate the variability in the quality of Rhubarb. Methods: Solutions of bofutsushosan extract products, bofutsushosan decoction, and Rhubarb decoction were subjected to solid‐phase extraction, and then were analyzed using HPLC. The five Rhubarb extracts prepared from five different lots were subjected to NMR‐based metabolomics analysis. Results: The quantities of sennosides A and B varied among the bofutsushosan extract products, with a maximum interproduct variation of approximately five‐fold. Sennosides A and B were not significantly unstable to heat up to 60 min. The five Rhubarb samples were classified into three independent clusters. Conclusion: It is recommended that the quantities of sennosides A and B in Kampo extract products, including Rhubarb, be described in the package insert. When preparing Rhubarb‐containing Kampo medicines, sennosides A and B decomposition can be ignored for decoction times of up to 60 min. Further studies on the biological activity of secondary metabolites other than sennosides A and B are necessary for Rhubarb quality control. [ABSTRACT FROM AUTHOR]

Advancing our understanding of dissolved organic matter (DOM) chemistry in aquatic systems necessitates the integration of data streams from multiple analytical platforms. Some measurements require pretreatment with solid phase extraction (SPE), while others are performed directly on whole water samples. Evidence has suggested that SPE will be biased against select DOM fractions, leading to concerns over the ability to establish data linkages across platforms with variable needs for SPE pretreatment, such as those from optical measurements and those that provide high‐resolution molecular information. Here, we directly addressed this concern by assessing the impact of SPE on DOM optical properties through excitation–emission matrices with parallel factor analysis (PARAFAC) for 47 samples across a stream network within a single watershed reflective of variable DOM sources. PARAFAC data was further paired with molecular information obtained by Fourier transform ion cyclotron resonance mass spectrometry (FTICR‐MS). A comparison of PARAFAC models first revealed no systematic qualitative differences in major components between whole water DOM and DOM isolated by SPE (SPE‐DOM); however, quantitative biases against select components were observed. Further linkages with FTICR‐MS data revealed that the molecular fingerprint associated with each PARAFAC component was consistent between the whole water DOM and SPE‐DOM. Our results suggest that bulk scale linkages across these analytical platforms could be inferred irrespective of the observed quantitative biases resulting from SPE for samples within this example watershed. This work represents a key step toward the systematic evaluation of linkages between optical and high‐resolution mass spectrometry datasets in freshwater lotic environments. [ABSTRACT FROM AUTHOR]

Rationale: Secondary hypertension is often caused by activation of complex multi‐organ endocrine systems, while renin activity indicated by angiotensins (Angs), aldosterone (ALD) and cortisol (COR) in such systems are generally accepted as its diagnostic markers. As antibody‐based methods cannot offer comparable quantification for these biomarkers, a liquid chromatography (LC)–tandem mass spectrometry (MS/MS)‐based approach was developed to quantify them simultaneously and accurately. Methods: Five different beads for magnetic solid‐phase extraction (MSPE) were evaluated towards their enrichment efficiency for these biomarkers. An LC system with optimized elution gradient and a triple‐quadrupole MS with tuned parameters were coupled to quantitatively monitor the extracted analytes. The method performance was further examined such as linearity, precision, stability, recovery rate and matrix effect. Based on the developed method, the abundance of Ang II, ALD and COR in plasma was measured and the quantification was compared with that derived from commercial ELISA kits. Results: As compared with other MSPEs, Angs, ALD and COR were highly enriched by the HLB magnetic beads with satisfactory recoveries. These analytes were simultaneously quantified by LC/MS/MS and all the method parameters for quantification were well matched with the requirements of clinical testing. Comparison of the quantitative results derived from ELISA and LC/MS/MS exhibited that the two methods offered basically comparable values with Pearson r values at 0.896, 0.895 and 0.835, respectively. The stability test for plasma Angs at room temperature indicated that the abundance of Ang II was relatively stable within 3 h, whereas that of Ang I and Ang 1–7 was time‐dependently changed. Conclusions: Coupling of HLB beads and LC/MS/MS thus enables simultaneous quantification of a set of biomarkers related to secondary hypertension. [ABSTRACT FROM AUTHOR]

Rationale: The volatile organic compounds (VOCs) of Lonicerae Japonicae flos (LJF) and Lonicera flos (LF) play a pivotal role in determining their sensory characteristics, medicinal properties, and subsequent impact on market pricing and consumer preferences. However, the differences and specificity of these VOCs remain obscure. Hence, it is crucial to conduct a comprehensive characterization of the VOCs in LJF and LF and pinpoint their potential differential VOCs. Methods: In this study, headspace gas chromatography–ion mobility spectrometry (HS‐GC/IMS) and headspace solid‐phase microextraction gas chromatography–mass spectrometry (HS‐SPME‐GC/MS) were employed to comprehensively investigate the compositional characteristics and distinctions in VOCs between LJF and LF. Multivariate statistical analysis was used to identify candidate differential VOCs of LJF and LF samples. Results: A total of 54 and 88 VOCs were identified using HS‐GC/IMS and HS‐SPME‐GC/MS analysis, respectively. Primary VOCs detected in LJF include leaf alcohol, (E)‐2‐hexen‐1‐ol dimer, 2‐octyn‐1‐ol, and (E)‐3‐hexen‐1‐ol. Key VOCs prevalent in LF encompass farnesol, heptanoic acid, octanoic acid, and valeric acid. Multivariate statistical analysis indicates that compounds such as phenethyl alcohol and leaf alcohol were selected as potential VOCs for distinguishing between LJF and LF. Conclusion: This research conducted a comprehensive analysis of the fundamental volatile components in both LJF and LF. It subsequently elucidated the distinctions and specificities within their respective VOC profiles. And this study enables differentiation between LJF and LF through the analysis of VOCs, offering valuable insights for enhancing the quality control of both LJF and LF. [ABSTRACT FROM AUTHOR]

Due to an outbreak of coronavirus spreading in recent years, there is an urgent need for effective, rapid, and non‐invasive diagnostics to detect and differentiate among patients who are infected and uninfected with SARS‐CoV‐2 for controlling the virus propagation. This study developed an alternative method for COVID‐19 screening from volatile analysis of metabolites mainly studied in sweat samples obtained from the populations in Bangkok, Thailand, during December 2020 to April 2022. A total of 140 collected samples; 70 positive confirmed COVID‐19 cases and another 70 negatives confirmed COVID‐19 cases were applied to be separated, detected, and identified as volatile organic compounds (VOCs)/odor occurring from SARS‐CoV‐2 infection body by the technique of Headspace solid‐phase microextraction gas chromatography‐mass spectrometry (HS‐SPME‐GC‐MS) together with principle component analysis (PCA), which allowed potential volatile markers of COVID‐19 such as pentadecane, nonanal, styrene, xylene, ethylbenzene, and 2‐ethylhexyl acrylate (up to 94 % accuracy, 93 % sensitivity, 96 % selectivity, and 94 % specificity), respectively, along with limit of detection in a range of 0.26–125 μg. The result was validated by comparison with the RT‐PCR results. [ABSTRACT FROM AUTHOR]

Rationale: Osilodrostat is an inhibitor of 11‐beta‐hydroxylase (CYP11B) and is used for the treatment of Cushing's disease but also categorized as an anabolic agent. The use of osilodrostat is prohibited in horseracing and equestrian sports. To the best of our knowledge, this is the first metabolic study of osilodrostat in equine plasma. Methods: Potential metabolites of osilodrostat were identified by differential analysis using data acquired from pre‐ and post‐administration plasma samples after protein precipitation with liquid chromatography electrospray ionization high‐resolution mass spectrometry (LC/ESI–HRMS). [Correction added on 27 January 2023, after first online publication: In the preceding sentence, "C–HRMS" was changed to "LC/ESI–HRMS" in this version.] For quantification of osilodrostat, a strong cation exchange solid‐phase extraction was employed, and the extracts were analyzed using LC/ESI–triple quadrupole tandem mass spectrometry (LC/ESI–QqQ‐MS/MS) to establish its elimination profile. Such extracts were further analyzed using LC/ESI–HRMS to investigate the detectability of osilodrostat and its identified mono‐hydroxylated metabolite over a 2‐week sampling period. Results: Mono‐hydroxylated osilodrostat was identified based on the differential analysis and mass spectrometric interpretations, and it was found to be the most abundant metabolite in plasma. Elimination profile of osilodrostat in plasma was successfully established over the 24‐h post‐administration period. Both osilodrostat and its mono‐hydroxylated metabolite were detected up to the last sampling point at 2 weeks using HRMS, and osilodrostat could be confirmed up to 8‐day post‐administration with its reference material using HRMS as well. Conclusions: For doping control, screening of both the parent drug osilodrostat and its mono‐hydroxylated metabolite in equine plasma would be recommended due to their extended detection windows of up to 2 weeks. Given the availability of reference material for potential confirmation in forensic samples, osilodrostat is considered the most appropriate monitoring target. [ABSTRACT FROM AUTHOR]

There is a strong interest in monitoring copper in environmental waters, but its direct analysis suffers from strong matrix interferences. This is why, a sample pretreatment based on solid‐phase extraction (SPE) is often used but conventional sorbents usually lack specificity. It is overcome with ion‐imprinted polymers (IIPs). This work evaluates for the first time the use of the dummy approach for the synthesis of Cu(II)‐targeting IIPs. Two analog ions Ni(II) and Zn(II) were tested as templates and the resulting IIPs were packed in SPE cartridges. The SPE procedure was designed by optimizing a washing step following the sample percolation, to eliminate the interfering ions retained on the IIP by non‐specific interactions. To optimize the washing step, solutions at different pH or containing tris(hydroxymethyl)aminomethane as a complexing agent at different concentrations were tested and combined. Zn‐IIP appeared more promising than Ni‐IIP, showing excellent specificity and a high selectivity. Its retention capacity was determined to be 100 µg/g, and different isotherm models were evaluated to fit with the adsorption data. Finally, applications to mineral and sea waters were successfully completed and led to high and repeatable extraction recoveries for Cu(II) (88 ± 1% and 83 ± 3%, respectively). [ABSTRACT FROM AUTHOR]

Here, a simple/efficient analytical strategy based on dispersive solid phase extraction was developed using CoSn(OH)6 nanocubes for lead ions from environmental water samples by FAAS (flame atomic absorption spectrometry). CoSn(OH)6 was synthesized as an adsorbent using the co‐precipitation method and characterized. The characterization studies proved the cube‐shaped morphology and uniform size distribution. The optimal experimental conditions were found by optimization studies and, the limit of quantification (LOQ), limit of detection (LOD), linear dynamic range were recorded as 37.6 μg/L, 11.3 μg/L, and 40–600 μg/L, respectively. The enhancement factor of the presented method was calculated as 158.7‐folds compared to the LOD of the conventional FAAS system. Recovery experiments were performed to check the method's applicability/accuracy and the percent recovery results varied from 89.0 % to 112.9 %. According to these findings, the developed method was successfully applied for the quantitative determination of the target analyte in a seawater sample matrix. [ABSTRACT FROM AUTHOR]

Solvent‐assisted dispersive solid‐phase extraction (SA‐DSPE) approach was developed to measure triazole fungicides (TFs). In the SA‐DSPE technique, the addition of 1000 μL of ethanol as a disperser solvent, along with a small quantity of benzil as a sorbent to the sample solution, led to a cloudy solution. After completion of the extraction, the mixture was subjected to centrifugation to isolate benzil. Next, benzil was dissolved in ethanol, and the resulting solution was subsequently analyzed by a gas chromatography‐flame ionization detector. This method demonstrated high linearity (R2 > 0.9963) and repeatability (relative standard deviation % < 4.3) for the quantification of TFs under the optimal conditions (sorbent: benzil, amount of benzil: 2% w/v, pH of solution: 7.0, disperser solvent: ethanol, volumes of ethanol: 1000 μL, centrifuge time: 3 min, extraction temperature: 25°C, and ionic strength: without salt addition). The proposed SA‐DSPE yielded detection limits, quantification limits, and preconcentration factors within the ranges of 0.3–0.9 ng/mL, 1.0–3.0 ng/mL, and 419–426, respectively. Finally, the validated method was employed to determine TFs in a diverse range of real samples, encompassing waters, fruits, vegetables, and agricultural soils, with relative recoveries ranging from 93.0% to 104%. [ABSTRACT FROM AUTHOR]

Anchoring an imidazole‐di‐tert‐butyl‐arylsilane possessing an azido group to a polystyrene resin provided a heterogeneous precursor that was radiolabeled easily using aqueous [18F]fluoride. After optimizing the conditions (i.e., using DMSO as solvent and heating at 160°C for 15 min), the desired [18F]fluorosilane was obtained in 24% radiochemical yield (RCY) and 78% radiochemical purity (RCP) using solid‐phase extraction as sole purification. Then, this compound was conjugated by strain‐promoted alkyne–azide cycloaddition to a model single‐variable domain possessing a cyclooctyne tag, yielding to the desired 18F‐labeled bioconjugate in 2% RCY and >95% RCP after purification by a size exclusion chromatography. [ABSTRACT FROM AUTHOR]

In this work, monodisperse and nano‐porous poly(bismaleimide‐co‐divinylbenzene) microspheres with large specific surface area (427.6 m2/g) and rich pore structure were prepared by one‐pot self‐stable precipitation polymerization of 2,2′‐bis[4‐(4‐maleimidophenoxy) phenyl] propane and divinylbenzene. The prepared poly(bismaleimide‐co‐divinylbenzene) microspheres were employed as dispersive solid‐phase extraction (DSPE) adsorbent for the extraction of triazine herbicides. Under optimized conditions, good linearities were obtained between the peak area and the concentration of triazine herbicides in the range of 1–400 µg/L (R2 ≥ 0.9987) with the limits of detection of 0.12–0.31 µg/L. Triazine herbicides were detected using the described approach in vegetable samples (i.e., cucumber, tomato, and maize) with recoveries of 93.6%–117.3% and relative standard deviations of 0.4%–3.5%. In addition, the recoveries of triazine herbicides remained above 80.7% after being used for nine DSPE cycles, showing excellent reusability of poly(bismaleimide‐co‐divinylbenzene) microspheres. The adsorption of poly(bismaleimide‐co‐divinylbenzene) microspheres toward triazine herbicides was a monolayer and chemical adsorption. The adsorption mechanism between triazine herbicides and adsorbents might be a combination of hydrogen bonding, electrostatic interaction, and π‐π conjugation. The results confirmed the potential use of the poly(bismaleimide‐co‐divinylbenzene) microspheres‐based DSPE coupled to the high‐performance liquid chromatography method for the detection of triazine herbicide residues in vegetable samples. [ABSTRACT FROM AUTHOR]

Mycotoxin contamination is widespread in plants and herbs, posing serious threats to the consumer and human health. Of them, alternariol (AOH) has attracted great attention as an "emerging" mycotoxin in medicinal herbs. However, a specific and high‐throughput extraction method for AOH is currently lacking. Thus, developing an efficient pre‐treatment technique for AOH detection is extremely vital. Here, a novel automated magnetic solid‐phase extraction method was proposed for the highly efficient extraction of AOH. Combining the aptamer‐functionalized magnetic nanoparticles (AMNPs) and the automatic purification instrument, AOH could be extracted in medicinal herbs in high throughput (20 samples) and a short time (30 min). The main parameters affecting extraction were optimized, and the method was finally carried out by incubation AMNPs with 3 mL of sample solution for 10 min, and then desorption in 75% methanol for liquid‐phase detection. Under optimal conditions, good reproducibility, stability, and selectivity were realized with an adsorption capacity of 550.84 ng/mg. AOH extraction in three edible herbs showed good resistance to matrix interference with recovery rates from 86% to 111%. In combination with AMNPs and the automatic purification instrument, high‐throughput and labor‐free extraction of AOH in different complex matrices was achieved, which could be extended in other complex matrices. [ABSTRACT FROM AUTHOR]

Multiwalled carbon nanotubes (MWCNTs) are well‐known adsorbents because of their high surface area, layered and hollow architecture, hydrophobicity, and multiple and easily accessible adsorption sites. In this study, MWCNTs were used for dispersive micro‐solid‐phase extraction of various metal chelates in environmental and food samples. Different parameters such as concentration of the chelating reagent, the sorbent dosage, the extraction time, the desorption time, and the strength of the eluent were suitably optimized. Under the optimum extraction conditions, the proposed method demonstrated a good linear working range for all the analytes, with correlation coefficients above 0.9915. The limit of detection ranged from 0.02 to 0.21 μg/L. The inter‐day and intra‐day relative standard deviations were less than 2.5 %. The proposed method was used for the determination of selected metals in tap water, drinking water, cucumber, and tomato samples. In the end, GAPI tool was used to evaluate the greenness of the method. [ABSTRACT FROM AUTHOR]

A novel silica fabricated allyloxy ethanol based imprinted polymer is synthesised with surface area of 333 m2 g−1 and average pore size of 6.5 nm by an environment friendly one pot surface imprinting process. It was employed for the selective solid‐phase extraction (SPE) of trace Ni(II) in real samples prior to FAAS determination. The factor settings produced via central composite design in response surface methodology (RSM) (pH: 3.6; initial concentration; 800 mg L−1 and time; 15 minute) provide adsorption capacity of 176 mg g−1. Artificial neural network model employed on the RSM data, provided better predictability. Sips isotherm model and BSf kinetic model describes best the sorption phenomena of the homogenous binding terrain. The developed SPE‐coupled FAAS method demonstrate a detection limit of 1.62 μg L−1, quantification limit of 4.17 μg L−1, and Linear dynamic range of 20–8000 μg L−1. It was successfully applied to determine nickel in food (Spinach, Radish, Green tea infusion, Black tea infusion, Coffee, Soya milk, Chocolate Soya milk, Tobacco) and wastewater samples (>99 % removal). For five replicate determinations, the method's relative standard deviation was 2.3 %. The method was validated by analysing two certified reference materials, and the outcomes were well‐congruent with standard values. For the synthesised polymer Ni(II) exhibits higher distribution ratio than other competing ions (Cu(II), Pb(II), Cd(II), and Zn(II)) with the imprinting factor; β values of 5.73, 4.98, 6.80, and 5.04 respectively. The reusability experiments revealed that APS@Ni‐IIP retains a strong adsorption efficacy even after 15 cycles and after its exhaustion it was employed as catalyst for reducing permanganate ions, further reducing pollution. The rigid structure of mesoporous silica contributes to its acid resilience and reusability, which can lead to a relative increase in polymer performance in absorption rate and selectivity. Apart from the novelty in the synthesis, thorough examination of the method and material selectivity (in binary, ternary and multielement system), multi fold applications of determination, removal of Ni(II) and reduction of permanganate ions, makes APS@Ni‐IIP a promising candidate for environmental remediation. [ABSTRACT FROM AUTHOR]

Restricted access materials (RAMs) with adjustable selectivity was developed for the removal and detection of residual dyes for the solve problems of dye contamination. In this work, using homemade poly(4‐vinylbenzyl chloride‐co‐divinylbenzene) (PVBC/DVB) microspheres as substrate and successive two‐step surface‐initiated atom transfer radical polymerization (SI‐ATRP) as synthesis method, the two types of monomers, sodium 4‐vinylbenzene sulfonate (Nass) and styrene (St) were first grafted for constructing mixed interactions of adsorption sites, and then the hydrophilic glycidyl methacrylate (GMA) was polymerized, following by hydrolysis to construct diol groups on the external PVBC/DVB as the restricted access sites. The developed PVBC/DVB@poly(St‐co‐Nass)@poly(GMA) of adsorption properties was investigated by six dyes including methylene blue (MB), basic fuchsin (BF), acid fuchsin (AF), neutral red (NR), methyl orange (MO), and Congo red (CR), the adsorption capacities of those dyes and the removal rate for the binary mixed dye solution both rely on the ratio of St/Nass, confirming the adjustable adsorption selectivity. When PVBC/DVB@poly(St‐co‐Nass)@poly(GMA) was packed as solid phase extraction adsorbent in couple with UV–vis spectrum, it was applied to the determination of MB and BF in the water, fish and shrimp, good linearity with satisfactory recoveries for MB and BF are obtained to show the favorable practicability. [ABSTRACT FROM AUTHOR]

In this study, eight pharmaceuticals belonging to two classes, antihistaminic and antimigraine, were considered. Ultra‐performance liquid chromatography‐diode array detection was set up and gradient elution was used. The mobile phase was composed of acetonitrile and trifluoroacetic acid solution. Chromatographic separation was carried out with a run time of 9 min. The preconcentration of eight studied solutes was realized by micro solid‐phase extraction. Multiwalled carbon nanotubes, cetyltrimethylammonium bromide‐titanium dioxide nanotubes, and C‐18 bonded silica solid‐phase extraction (SPE) sorbents were evaluated and compared concerning recoveries. The results of the optimization of factors affecting the extraction efficiency including sample volume, the elution solvent type, and its volume are reported. For validation of the analytical procedure, specificity, linearity, precision, accuracy, limit of detection, and limit of quantification were evaluated. The developed method was successfully applied to the analysis of wastewater treatment samples. The extraction recoveries of pharmaceutical substances were above 81.23% for the three SPE sorbents. The extraction method was selective and the detection and quantification limits were between 0.004–0.02 and 0.01–0.06 μg/L, respectively. All the results indicated the potential application of the three studied SPE sorbents for the extraction of selected pharmaceuticals from wastewater. [ABSTRACT FROM AUTHOR]

An efficient analytical method has been developed based on dispersive solid‐phase extraction followed by gas chromatography‐mass spectrometry for the determinations of 13 organochlorine pesticides in fruit juice samples. In this method, dispersive solid phase extraction was used for the extraction of target analye using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent. Different experimental parameters affecting the extraction efficiencies the proposed method were carefully optimized. Under the optimum conditions, the calibration graphs were linear in the concentration range of 0.6–100 ng/mL with coefficients of determinations in the range of 0.9927–0.9991. The limits of detection and quantification determined as 3 and 10 times the signal‐to‐noise ratio were in the range of 0.01–0.03 and 0.6–1.0 ng/mL, respectively. Intra‐ and inter‐day precision studies of the proposed method, expressed as relative standard deviations, were in the range of 2.1%–9.2% and 2.2%–9.7%, respectively. The recoveries of the spiked fruit juices samples were in the range of 81.4%–105.1% with the corresponding relative standard deviations ranging from 1.0%–8.8%. In general, the proposed method demonstrated satisfactory analytical performance. Thus,it could be used as simple and attracive alternative method for the extraction of organochlorine pesticides from fruit juice sample and other related matrices. [ABSTRACT FROM AUTHOR]