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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.

This work describes the development of temperature-induced dispersive solid phase extraction (TI-DSPE) for the isolation and measurement of cobalt in food and water samples. The concentration of the preconcentrated cobalt ions was determined using flame atomic absorption spectrometry (FAAS). In TI-DSPE, the dispersion of the sorbent occurs by varying the temperature. The cobalt was complexed with 1-nitroso-2-naphthol and extracted with finely dispersed benzoic acid particles at 60 °C. The extraction efficiencies parameters were assessed and optimized, such as the mass of benzoic acid, dissolution temperature, solution pH, centrifugation conditions, and ionic strength. In the optimum conditions, the analytical curve was linear from 2.0 to 150.0 µg L−1, the limits of detection and quantification were 0.55 and 1.83 µg L−1 respectively, and the preconcentration factor was 50. Ten repeated measurements at 50.0 µg L−1 yielded a relative standard deviation (RSD) of 2.6% (n = 10). High extraction recoveries (96.5–102.5%) were obtained from the analysis of real samples. The validity of the developed procedure was confirmed by analyses of certified reference materials (QC-1187 and SPS-SW2). The results demonstrated that the developed method was simple, efficient, and cost-effective. [ABSTRACT FROM AUTHOR]

The use of pesticides is often regarded as a fundamental aspect of conventional agriculture. However, these compounds have gained recognition as some of the oldest and most widely employed xenobiotic contaminants, necessitating effective strategies for human biomonitoring. In this context, a method was developed for the determination of 16 legacy organochlorine pesticides, 6 metabolites of current pesticides (2,4-D, malathion, parathion, fipronil, pyraclostrobin, cypermethrin, permethrin, cyfluthrin), and 1 triazine herbicide (atrazine) in serum. Samples were prepared with water, formic acid, acetonitrile, and ultrasound irradiation, followed by solid-phase extraction with Oasis Prime HLB. Subsequently, metabolites from current pesticides underwent derivatization using MTBSTFA with 1% TBDMSCl for analysis via gas chromatography-tandem mass spectrometry (GC–MS/MS), employing an SLB-5MS fused silica capillary column. Analytical curves were generated with limits of quantification from 0.3 to 4.0 ng.mL−1. Accuracy ranged from 69 to 124%, and the coefficient of variation from 2 to 28%. Moreover, determining 1-(4-chlorophenyl)-1H-pyrazol-3-ol was suggested as a biomarker for pyraclostrobin biomonitoring. This analytical approach facilitated the determination of both legacy and metabolites of current pesticides in the same serum sample, presenting an interesting and cost-effective option for large cohorts, and multi-omics studies that evaluate time-dependent biomarkers in blood samples, thereby enabling biomonitoring within the same matrix. Furthermore, a proof-of-concept involving 10 volunteers demonstrated exposure to 9 pesticides at mean concentrations measured in ng mL−1, consistent with findings from various biomonitoring initiatives. [ABSTRACT FROM AUTHOR]

Dried blood spot (DBS) technique has become a new popular topic in anti-doping field in recent years due to its advantages of sample stability and easy operation. It can be employed as a supplementary method to routine urine analysis. However, the small volume of DBS samples (usually 10–20 μL) significantly reduces the application value of this technique. Therefore, the development of sensitive detection methods for the analysis of prohibited substances in DBS is particularly important. In this study, based on the characteristics of low molecular mass peptide (LMMP) drugs, systematic optimization strategies were utilized for the first time to establish a sensitive detection method for LMMPs in DBS. Without using DMSO to enhance mass spectrometry ionization efficiency of peptides, the limits of detection (LOD) ranged between 0.05 and 3.74 ng/mL, significantly better than the previously reported method (0.5–20 ng/mL). This method was validated according to the guidelines of the World Anti-Doping Agency (WADA), and corresponding post-administration study was conducted, demonstrating that the method could be applied to routine analysis of LMMP drugs in DBS. Moreover, since DMSO is not involved, this method also has the potential to simultaneously detect both LMMP and small molecular drugs. [ABSTRACT FROM AUTHOR]

This study focuses on the development of eco-friendly biobased adsorbents through a sustainable hydrothermal and freeze-drying synthesis process, utilizing cost-effective bio-sourced materials to minimize energy consumption and waste. The biobased adsorbents were elaborated using hydroxyethyl cellulose-ionic liquids and bentonite clay. The elaborated biocomposites were characterized using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy/attenuated total reflection (FTIR/ATR), thermogravimetric analysis (TGA), and electron microscopy-energy dispersive X-ray (SEM–EDX), Brunauer–Emmett–Teller (BET) and zeta potential (ZP). Structural analysis confirms the intercalation and incorporation of HEC-ILs polymeric chains into Be-Na matrix and the formation of biocomposites. The [HEC-ILs/Be-Na] composite was subsequently employed for solid-phase extraction of Co(II) by investigating the effect of pH, initial Co(II) concentrations, time, temperature, and the presence of co-existing ions (Na(I), Li(I), Mn(II), Ni(II), and Al(III)). The adsorption kinetics of Co(II) metal ions were suitably characterized using the pseudo-second-order model (with R2 > 0.99). Furthermore, the adsorption isotherms conformed to the Langmuir model (with R2 > 0.97), suggesting a chemisorption process with an adsorption capacity of 69.8 mg/g. The thermodynamic study reveals that the adsorption process exhibits characteristics of spontaneity and endothermicity (ΔH° = 74.197 kJ mol−1, ΔG° < 0 kJ mol−1). The proposed mechanism for Co(II) adsorption on the developed biocomposite involves electrostatic interactions, ion exchange, and anion-π interactions. The biobased composite exhibited remarkable selectivity for Co(II) and demonstrated great potential as an adsorbent for industrial applications. [ABSTRACT FROM AUTHOR]

Sample pretreatment is an essential procedure in pesticide analysis, as the matrix effect can significantly influence the results. In this study, a covalent organic framework (COF) was synthesized using 1,2,4,5-tetrakis-(4-formylphenyl)benzene (TFPB) and benzidine (BD) to mitigate the matrix effect in vegetable and fruit samples. This COF was then used to develop a solid-phase extraction (CSPE) method. In addition, the COF was used to create a magnetic COF (MCOF) for use in magnetic solid-phase extraction (MSPE). The synthesized COF and MCOF were thoroughly characterized using scanning electron microscopy (SEM) for morphological analysis, Fourier-transform infrared spectroscopy (FT-IR) for chemical bond identification, and N2 adsorption–desorption measurements for porosity and surface area assessment. Key pretreatment parameters such as buffers, dilution rate, sorbent dosage, extraction time, elution solvent, and reuse number were optimized. The developed CSPE and MSPE showed excellent purification ability for the matrix of vegetable and fruit samples. The reuse test demonstrated that the synthesized COF and MCOF can be reused up to 15 times. Moreover, the developed CSPE and MSPE showed acceptable recoveries in spiked recovery tests, suggesting that these pretreatment methods were feasible for sample purification in pesticide analysis. [ABSTRACT FROM AUTHOR]

Methamphetamine, pseudoephedrine, and related drugs are among the first drugs used for the stimulation of the central nervous system. In this study, two adsorbents based on graphene oxide (GO) were synthesized and used for the analysis of methamphetamine and pseudoephedrine. The prepared nano-adsorbents based on GO in this study were coated by polyaniline (PANI) and Fe3O4/C-nanodot/GO (magnetic adsorbent). The average size of nanoparticles (GO/PANI) was 18.43 nm. The specific surface area and pore size diameter of Fe3O4/C-nanodot/GO were 22.71 m2 g− 1 and 15.23 nm, respectively. Experimental variables affecting the extraction efficiency of the analytes such as pH of the sample solution, amount of adsorbent, extraction time, and type of eluents were investigated and optimized by response surface methodology. Under optimum conditions, GO/PANI and Fe3O4/C-nanodot/GO were considered appropriate solid phase extraction adsorbents for HPLC-based analyses of the studied drugs in human urine samples. However, GO/Fe3O4 nano adsorbent (Fe3O4/C-nanodot/GO) showed superior working condition than GO/PANI. The validated proposed analytical methods can be used for the quantitative determination of methamphetamine and pseudoephedrine in actual samples. [ABSTRACT FROM AUTHOR]

AbstractA flow injection (FI) method employing the reaction between 1,10-phenanthroline (C12H8N2) and hydrogen peroxide (H2O2) in a basic medium (pH 12) with chemiluminescence (CL) detection has been developed to detect copper oxychloride pesticides in freshwater and fruit samples. The experimental conditions were optimized, and a solid phase extraction (SPE) technique modified with cupron was employed for effective phase separation during extraction. Calibration curves for copper oxychloride standard solutions demonstrated linearity over the range of 0.001 to 10 μg L−1, with the regression equation y = 506681x − 422.29 and a coefficient of determination (R2) of 0.9973 (n = 9). The limits of detection (LOD) and quantification (LOQ) were determined to be 2.62 × 10−4 μg L−1 and 7.94 × 10−4 μg L−1, respectively. Relative standard deviations (RSDs) ranged from 2.6% to 4.5%, and the method achieved an injection throughput of 120 h−1. When applied to spiked water and fruit samples, the method showed no significant differences at the 95% confidence level compared to established methods. Recoveries for copper oxychloride were found to range from 96% to 120% (RSD = 1.9 − 5.6%) in fruit samples and from 95% to 110% (RSD = 1.5 − 4.8%) in water samples. Additionally, the potential chemiluminescence reaction mechanism was investigated. [ABSTRACT FROM AUTHOR]

In this study, we designed a molecularly imprinted polymers-dispersive solid-phase extraction-high-performance liquid chromatography (MIPs-DSPE-HPLC) method, as a simple and efficient platform for the sensitive detection of two sulfonamide antibiotics (SAs) of sulfamethoxine (SMM) and sulfamethoxazole (SMZ) in environmental water samples. Using SMM and SMZ as templates, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the crosslinking agent, and azodiisobutyronitrile as the catalyst, the dual-template molecularly imprinted polymers (dt-MIPs) were successfully synthesized via surface imprinting technology and multi-template imprinting strategy. The adsorption properties of the prepared MIPs were characterized, and the adsorption capacities of MIPs towards SMZ and SMM were 27.35 mg/g and 30.92 mg/g, respectively. The detection limits of the method in three environmental water samples were in the range of 0.23–1.74 μg/L, and the recoveries were between 82.7 and 110.3%, with relative standard deviations less than 5.93%. The construction process of this MIPs-DSPE-HPLC method is straightforward, exhibits high sensitivity and selectivity, and thus provides a versatile method for the quantification of SAs in complex matrices. [ABSTRACT FROM AUTHOR]

In the present study, a modified carbon nano-onion and β–cyclodextrin composite was utilized in micro-solid phase extraction of atenolol and metoprolol from human plasma samples. The synthesized sorbent structure and morphology were evaluated. In this method, a proper amount of the sorbent was contacted with the diluted plasma sample under vortexing (to promote the sorbent contact area with the solution). The separated particles by centrifugation were contacted with a proper eluent to desorb the target analytes. After that, the eluent was separated by centrifugation and used during analysis of the analytes by high-performance liquid chromatograph. Several effective extraction parameters such as the sorbent amount, type and elution solvent volume, and extraction time were evaluated and optimized. The validated factors showed that detection and quantification were 0.09 and 0.01 and 0.29 and 0.03 ng mL–1, for metoprolol and atenolol, respectively. The method precision, considered as relative standard deviation, was ≤ 2.5 and ≤ 3.6% for intra- (n = 5) and inter-day (n = 4) precisions, respectively. The extraction recovery values were obtained 84 and 63% for metoprolol and atenolol, respectively. Lastly, the developed method was utilized successfully on the plasma samples of patients treated with metoprolol and atenolol. [ABSTRACT FROM AUTHOR]

Selenium (Se) is considered to be an essential trace element needed for all living organisms. The importance, deficiency, and toxic effects of Se mainly depend on its quantity and chemical nature. It has been observed that the inorganic versions of Se are more hazardous than the organic versions. This review is mainly focused on the application of different extraction methods used for Se extraction and determination such as microextraction, solid-phase extraction (SPE), and their modified modes in the last 12 years. The use of different dispersive medium (magnetic field, ultrasonic radiation, and vortex agitator) to enhance Se separation is also part of this review. The usage of environmentally friendly solvents such as supramolecular solvents, hydrophobic deep eutectic solvents (DESs), and ionic liquids (ILs) are also the focus of attention in this review. This review is also emphasized the application of advanced microextraction methods, particularly liquid-phase microextraction (LPME). The most recent advances in LPME extraction techniques for Se in various environmental samples, as well as their prospects, are reviewed. Additionally, a summary of cheap, simple, and accurate techniques that have not yet been used to determine small amounts of Se has been provided. [ABSTRACT FROM AUTHOR]

In the current study, a solid phase extraction (SPE) methodology utilizing sodium ferrite nanoparticles (Na2Fe4O7-NPs; SF-NPs) is presented for the simultaneous determination of heavy metals (HMs) via flame atomic absorption spectrometry (FAAS). SF-NPs were synthesized by an eco-friendly sol–gel auto-combustion method using Tamarindus indica fruit extract as a stabilizing agent. The characterized SF-NPs exhibited a high surface area with uniform distribution, high stability, and a negative surface charge, making it a promising material for excellent adsorption of HMs. The SF-NP-based SPE procedure involved optimizing parameters such as pH, adsorbent dosage, sample volume, eluent composition, volume, and concentration. The developed SF-NP-based SPE method demonstrated low detection limits, i.e., 0.006, 0.008, and 0.009 μg L−1 for the analysis of Cd, Cu, and Pb, respectively. The SF-NP-based SPE methodology was validated by examining certified reference material and real samples, yielding accurate results with good recoveries (>95%) with a relative standard deviation of <5.0%. The developed SF-NP-based SPE method offers a promising approach for the simultaneous determination of Cd, Cu, and Pb in water and food samples, providing an efficient and environmentally friendly analytical tool for monitoring heavy metal contamination. [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 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]

This study aims to statistically compare two methods for determining 210Pb in tobacco: the molecular recognition sorbent method (AnaLig Sr01) and the extraction chromatography sorbent method (Sr Resin). The TriCarb 3100 TR liquid scintillation spectrometer was used to measure and determine 210Pb activity in the tobacco solution. Statistical analysis confirmed the accuracy and precision of the 210Pb measurements, with high detection efficiencies of 82% for both AnaLig Sr01 and Sr Resin. The linear model demonstrated that the residuals followed the Gaussian model, without any autocorrelation or trend. Paired t tests showed consistent results across all methods, and all solid-phase extraction methods proved efficient for 210Pb separations in tobacco samples. These findings provide support for the suitability of both methods and lay a foundation for future articles on tobacco and cigarette samples. [ABSTRACT FROM AUTHOR]

Clozapine (CLZ) -related accidents or crimes are common in the world. Oral fluid drug detection is a convenient measure of dealing with things like that. There has not been any literature reported detailedly the representation rule of clozapine and its metabolites in oral fluid so far. The study aimed to describe the pharmacokinetics of CLZ and its metabolites N-desmethylclozapine and clozapine-N-oxide in human oral fluid after a single 12.5 mg oral dose of CLZ. Twenty-nine volunteers, including 20 males and 9 females, were recruited, and 2 mL oral fluid was collected from each participant at post-consumption time-points of prior (zero), 0.5, 1.5, 3, 5, 8, 12, 24, 36, 51, 82, and 130 h, respectively. Analytes of interest were extracted with solid-phase extraction and analyzed with liquid chromatography tandem mass spectrometry method. Pharmacokinetic parameters were calculated using the pharmacokinetic software DAS according to the non-compartment model. The maximum concentration, the time of maximum concentration, oral clearance, and the elimination half-life of clozapine were 16.57 ± 9.63 ng/mL, 4.53 ± 3.61 h, 57.65 ± 23.77 L/h and 53.58 ± 52.28 h, respectively. The maximum concentration, the time of maximum concentration, and the elimination half-life of the metabolite N-desmethylclozapine were 3.08 ± 1.19 ng/mL, 9.38 ± 9.33 h and 62.67 ± 82.57 h, respectively; of clozapine-N-oxide were 1.15 ± 0.36 ng/mL, 4.53 ± 2.19 h and 19.15 ± 23.11 h, respectively. It was the first study on the pharmacokinetics of CLZ and its metabolites in the oral fluid of Chinese healthy volunteers, and it provided a basis for the therapeutic drug monitoring and toxicological interpretation in clozapine-related cases. [ABSTRACT FROM AUTHOR]

Current study is based on the synthesis and characterisation of MgSiO3 nanoparticles (MgSiO3 NPs) and its application for ultrasound-assisted solid-phase extraction (UASPE) of methylene blue (MB) dye from water samples using UV-Vis spectrophotometry. The prepared MgSiO3 NPs were fully identified and characterised by different techniques such as Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Scanning electron microscope (SEM) and Energy-dispersive X-ray spectroscopy (EDS). The prepared nano sorbent had spherical shape with size diameter of 20 nm. Central composite design (CCD) optimisation approach as versatile tool was used for investigation and optimisation of the effective parameters. Using CCD method, the optimised conditions were achieved to be pH of 7.0, sorbent dosage of 29.80 mg, ultrasonic time of 10.34 min, and temperature of 25°C at 500 µl of dimethylformamide eluent using Triton X-100 surfactant. Under the optimised conditions, the proposed method is applicable for wide linear range with detection limit of 0.084 mg L−1, limit of quantification of 0.28 mg L−1. The prepared MgSiO3 NPs have exceptional properties in terms of porous and sheets structure and also high adsorption capacity. In addition, the applied method showed satisfactory figure of merits in terms of pre-concentration factor of 10, which make candidate the applied method and nano sorbent as an operative and ideal candidate for pre-concentration and determination trace level of MB from water samples. [ABSTRACT FROM AUTHOR]

A simple and sensitive magnetic solid phase extraction (MSPE) method was developed for the separation-preconcentration and speciation of Cr in water samples. The system is based on the adsorption of Cr (VI)-ammonium pyrrolidinedithiocarbamate (APDC) complex on the activated charcoal@MoSe2@Fe3O4 composite. Total chromium has also been determined after the conversion of Cr (III) to Cr (VI) by oxidation with KMnO4. Cr (III) was determined as the difference between the total content of the Cr and Cr (VI). For quantitative recoveries, the effects of solution pH, adsorbent amount, volume of the sample, ligand volume, eluent type, and volume and effect of foreign ions were investigated. The limit of detection and limit of quantification for Cr was 0.36 ng mL−1 and 1.19 ng mL−1, respectively. The procedure was applied for the determination and speciation of chromium in water samples. [ABSTRACT FROM AUTHOR]

Wine vinegar, valued for its ancient origins and culinary versatility, has garnered scientific interest due to its complex composition and potential health benefits. This study aims to explore the nutritional and bioactive properties of different wine vinegars, focusing on their amino acid content, particularly tryptophan-derived molecules such as serotonin and melatonin. White wine vinegar, red wine vinegar, port wine vinegar, and balsamic vinegar from the Douro and Rioja regions were analyzed using high-performance liquid chromatography and solid-phase extraction (HPLC-SPE). The study examined the amino acid profiles and the presence of serotonin and melatonin across the samples. The analysis revealed the presence of significant bioactive amino acids, including arginine (found in sample 059 at 61.21 mmol/L), alanine (in a concentration of 30.33 mmol/L in sample 209), and threonine (sample 336 presented the highest concentration—71.47 mmol/L), which have been linked to cardiovascular health, immune system support, and mucosal regulation. The amino acid content varied among the vinegar types, with slower acetification and prolonged aging reducing their concentrations. Tryptophan was mainly found in sample 059 (30.54 mmol/L). These findings, with their potential to influence the scientific community's understanding of the health-promoting properties of wine vinegar, particularly its amino acid content and the potential influence of production processes on bioactive molecules, are of great interest. [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]

Nitrosamines and semi-volatile organic compounds (SVOCs) are carcinogenic contaminants in water and biological matrices. Conventional analytical methods often struggle to detect trace concentrations due to poor extraction efficacies. This study presents a novel, low-cost, in-syringe-assisted fast extraction cum cleanup technique coupled with GC-FID for monitoring four nitrosamines and two SVOCs in drinking water and human urine samples to measure the contamination and exposure levels. This extraction protocol combines a novel green in-syringe liquid–liquid extraction step using dimethyl carbonate as the green extraction solvent, coupled with a semi-automated solid-phase extraction cleanup process. Then, the final extractant is analyzed using gas chromatography-flame ionization detection (GC-FID) for monitoring. The method demonstrated excellent linearity (R2 > 0.998) between 1.5 and 500 ng mL⁻1 for all six target compounds. Detection limits ranged from 1.0 to 2.0 ng mL⁻1. Extraction recoveries were between 87 and 105% for both urine samples and water samples. Intra-day and inter-day precision were below 9% RSD. The blue applicability grade index evaluation scored 70.0, indicating good practical applicability. The developed analytical protocol offers a sensitive, accurate, low-cost, rapid, and environmentally friendly method for simultaneously quantifying multiple nitrosamines and SVOCs in environmental and human samples. Its performance characteristics and sustainability metrics suggest the potential for broad application in monitoring and exposure studies. [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]

The chemical composition, including volatile metabolites of green coffee beans, is influenced by geographic origin. The aim of this study was to reveal the volatile metabolite profile of a single variety of Robusta green bean coffee from five major plantation regions in West Java and to correlate these profiles with temperature, rainfall, and altitude. By using solid phase micro extractions and gas chromatography‐mass spectrometry, 143 different volatile compounds were detected, with aromatic hydrocarbon, alcohols, monoterpene, pyrazines, sesquiterpenes, carboxylic acids, and terpene the most dominant. Principal component analysis (PCA) indicated 64.3% variability, showing that the metabolite profile of Robusta green coffee from the Bogor region was distinctly different from those in Ciamis, Kuningan, Sumedang, and Tasikmalaya, which were more similar to each other. Metabolites such as benzaldehyde, isovaleric acid, toluene, diisobutyl succinate, 1‐heptene, 4‐dodecene, caffeine, acetic acid, and methyl benzoate were identified as key discriminants, with a VIP score greater than 1.5. Temperature increases were linked to higher levels of isovaleric acid, diisobutyl succinate, 4‐dodecene, toluene, and acetic acid, while other discriminant metabolites declined. Increased rainfall was associated with higher levels of benzaldehyde, 1‐heptene, caffeine, and methyl benzoate, but lower levels of the other discriminants. Altitude had a positive correlation with methyl benzoate and 1‐heptene, and a negative correlation with isovaleric acid and 4‐dodecene, with weaker correlations for other compounds. In summary, Robusta green coffee beans from different regions of West Java can be distinguished by their volatile metabolites. Bogor green coffee beans had higher levels of benzaldehyde, 1‐heptene, caffeine, and methyl benzoate, Kuningan beans had more diisobutyl succinate and 4‐dodecene, Ciamis beans had higher levels of isovaleric acid, diisobutyl succinate, and 4‐dodecene, while Sumedang and Tasikmalaya beans were similar, with higher levels of isovaleric acid, diisobutyl succinate, 4‐dodecene, toluene, and acetic acid. This difference is related to the climatic factors of temperature and rainfall, as well as the altitude at which Robusta coffee is grown. [ABSTRACT FROM AUTHOR]

AbstractStatins are the most prescribed drug for regulating the high cholesterol level in the blood, which can lead to severe complications, such as cardiovascular diseases and other health complications. A wide range of analytical techniques have been employed for the quantification of statins from various origins, including fermentation derived (lovastatin, pravastatin, and compactin), semi-synthetic (simvastatin), and synthetic (atorvastatin, rosuvastatin, and fluvastatin) routes. The presence of more than one structural form and structural analogue generated in the biosynthesis pathway, as well as reaction intermediates and macromolecules in the clinical sample, complicates the quantification of statins. Furthermore, significant concentrations of statins in environmental samples pose serious health and ecology hazards, and estimating statins in those diluted samples is extremely difficult. On the other hand, the: cost, accurate estimation of the desired one from other structural forms, sample complexity, time, limits of detection and quantification, were major criteria distinguishing the usability of each technique. As a result, the current manuscript focuses on analytical techniques such as molecular spectroscopy (normal and derivatives UV-Visible spectrophotometer), chromatography (TLC, HP-TLC, HPLC, GC, swing column, micellar, and supercritical fluid), mass spectroscopy (HPLC-MS/MS and GC-MS/MS), sequential flow injection, capillary electrophoresis, and cyclic voltammetry, as well as their: optimal operating conditions, limits of detection and quantification, advancements, and limitations. Furthermore, various online and offline sample preparations (precipitation, solid phase extraction, liquid-liquid extraction, and micellar extraction) have been highlighted as an essential pretreatment technique to avoid the interference caused by structural analogues and other macromolecules. The greener and more sustainable concepts used in analytical approaches for the quantification statins are also highlighted with current advancements. [ABSTRACT FROM AUTHOR]

The solid phase extraction of Au, Ir, Pd, Pt, and Rh on a polymer gel modified with ionic liquid containing methylimidazolium groups (MIA-PG) has been investigated. The positively charged surface of the sorbent is highly suitable for the sorption of stable chlorido complexes of the studied analytes, while the retention of base metals Cu, Fe, Ni, Zn, and Mn is negligible. Optimization experiments performed showed that, at 0.05 M HCl, the degree of sorption of Au, Ir, Pd, and Pt is above 95%, and only for Rh, the maximum degree is 65%; complete elution is achieved in the mixture of thiourea in HCl. The results obtained from the equilibrium adsorption studies are fitted in various adsorption models, such as Langmuir and Freundlich, and the model parameters have been evaluated. The kinetics analysis indicated that the adsorption of Au, Ir, Pd, Pt, and Rh onto the sorbent follows the pseudo-second-order model. Intraparticle diffusion and ion exchange reactions were the rate-limiting steps. Analytical procedures were developed for Pd, Pt, and Rh determination in road dust and soil and for Au determination in copper ore and copper concentrate. The procedures are validated by the analysis of certified reference materials. Analytical figures of merit confirmed their applicability in routine laboratory practice. [ABSTRACT FROM AUTHOR]

A sorbent with magnetic properties, functionalized with humates, in combination with gas chromatography–mass spectrometry is proposed for the determination of phenolic xenoestrogens (ED) in bottom sediments. The octylphenol (OP), nonylphenol (NP), and bisphenol A (BPA) ED are chosen as test samples. Along with ED, the distribution of the naturally occurring estrogen, 17β-estradiol (ES), is studied. Sorption preconcentration is carried out under dynamic conditions: a sorbent weighing 0.5 g is placed in a borosilicate glass column, on both sides of which magnets are placed to immobilize the sorbent. The analytical characteristics of the determination method are established using model samples of bottom sediments selected in a background area with a minimal anthropogenic impact. The limit of quantification for ED is 30–60 ng/kg (dry weight). In analyzing real samples, the sensitivity of the method is reduced by 3–4 times due to matrix effects of the presence of petroleum products in waters. The ED content of bottom sediments at the site of wastewater discharge into the river Don near the city of Voronezh, as well as on the Black Sea coast of the Caucasus (area of the city of Tuapse and the village of Olginka) was monitored. The maximum concentrations of OP, NP, BPA, and ES in bottom sediments were found in the area of the port of Tuapse, where they were 5.7, 8.1, 6.2 and 0.9 µg/kg, respectively. [ABSTRACT FROM AUTHOR]

An original bench-scale installation based on the principles of online magnetic solid-phase extraction is developed. The setup includes a borosilicate glass column packed with Fe3O4@MIP-BPA, which is fixed with two neodymium magnets. Compared to using one magnet, a design with two magnets ensures the uniform distribution of the sorbent over the entire cross-section of the column. The highest concentration factors (EF = 3216) and the degree of desorption of bisphenol A (BPA) are achieved, respectively, at a volumetric solution flow rate (W) of 2.0 mL/min and with eluting BPA with methanol (W = 0.4 mL/min). The determination of BPA in concentrates from model media by GC−MS provides high sensitivity of the developed method for determining BPA. In analyzing model solutions prepared in distilled water, the limit of detection (LOD) is 0.3 ng/L. In analyzing river water, the LOD increases by approximately 2 times. In analyzing soils, LOD = 2.2 ng/kg dry weight. Soils, compared to water bodies, contain a larger number of interfering components; the sensitivity of the method is reduced by 7–8 times. Bottom sediments are even more contaminated; the LOD more than doubles compared to the determination of BPA in soils. [ABSTRACT FROM AUTHOR]

The adsorption of toxic ions Be(II), Bi(III), Cd(II), Cr(III), and Pb(II), and also noble metals Ag(I), Au(III), and Pd(II), from aqueous solutions is studied using carbon nanotubes (CNTs), a magnetic nanosorbent composed of CNTs and magnetic nanoparticles (CNT@MNP), and activated carbon (AC). An advantage of CNT-based adsorbents over AC in terms of capacity was demonstrated, with an increase of approximately 1.5–2 times. The adsorption capacity of the synthesized magnetic adsorbent depends on the morphology of CNTs grown on iron subgroup catalysts: nickel (CNT(Ni)), cobalt (CNT(Co)), and iron (CNT(Fe)). CNT@MNP exhibited superior performance over other carbon adsorbents in magnetic solid-phase extraction, effectively separating solid and liquid phases. Additionally, composite adsorbents containing CNT(Co) and CNT(Fe) were noted for their cost-effectiveness, as they yielded satisfactory results, surpassed those obtained with the individual CNT-based adsorbents. Procedures were developed using these carbon adsorbents and their performance in the determination of elements in aqueous solutions by arc atomic emission spectrometry was estimated. [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]

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.)

The unique flavour contribution of higher alcohols in alcoholic beverages has received growing attention; however, there is a dearth of information on their in vivo metabolic kinetics. In this study, the composition and content of higher alcohols in different alcoholic beverages from Chinese Baijiu and Lujiu were studied via in vivo analysis using Bama pigs to elucidate the mechanisms for intoxication of alcohol in vitro and in drinkers. Direct injection combined with gas chromatography–mass spectrometry (GC-MS) were used to accurately quantify a total of 14 higher alcohols in five alcoholic beverages. Based on the external standard method, a total content of 289.37–938.33 mg/L was detected, mainly 1-butanol, 3-methyl-1-butanol, 1-hexanol, 2-methyl-1-propanol and 2-butanol. Then, headspace solid-phase microextraction (HS-SPME) and solid-phase extraction (SPE) combined with GC-MS analysis strategy, respectively, were adopted to continuously monitor the changes in the concentrations of ethanol and 11 higher alcohols in the blood within 24 h after gavage of different alcoholic beverages, and the key pharmacokinetic parameters were analysed. The peak concentration (Cmax) and area under curve (AUC) of blood higher alcohols were significantly lower than those of ethanol (p < 0.05), accompanied by a later peak time (Tmax) and a larger apparent clearance rate (CL_F), and there were certain differences between the same higher alcohols in different alcoholic beverages and between different higher alcohols in the same alcoholic beverage. This work provides valuable insights into the metabolism of alcoholic beverages. [ABSTRACT FROM AUTHOR]

Marine dissolved organic matter (DOM) is an important, actively cycling carbon reservoir (662 GtC). However, the chemical structure and cycling of DOM within rapidly warming, polar environments remains largely unconstrained. Previous studies have shown rapid surface cycling of carbohydrates as biologically-labile DOM (LDOM). Conversely, carboxyl-rich alicyclic molecules (CRAM) are often used as examples of biologically-recalcitrant DOM (RDOM). Traditional DOM isolation methods (e.g., ultrafiltration (10–30% of DOM) and solid-phase extraction (40–60% of DOM) induce chemical-, size- and compositional-bias – complicating inferences to total DOM cycling. Here, we use a total DOM proton (1H) nuclear magnetic resonance (NMR) spectroscopy method to show carbohydrates and CRAM have high concentrations in the surface ocean and low concentrations at depth in Baffin Bay. Between 21–43% of surface CRAM is removed at depth. These results suggest both CRAM and carbohydrates are major LDOM constituents – contradicting the existing CRAM cycling paradigm and further constraining the long-term persistence of deep ocean DOM. A study using total dissolved organic matter (DOM) proton nuclear magnetic resonance spectroscopy found rapid removal of surface-derived carbohydrates and carboxyl-rich alicyclic molecules at depth, challenging our notions of deep ocean DOM storage. [ABSTRACT FROM AUTHOR]

AbstractA metal–organic framework (MOF-199) nanocomposite was coated on magnetic graphene oxide (MGO) as a sorbent (MGO/MOF-199) and used for the isolation of aromatic amines by magnetic solid-phase extraction (MSPE). The analytes subsequently determined using gas chromatography with a flame ionization detector (GC-FID). The sorbent mass, desorption solvent, extraction time, desorption time, and pH were optimized. The calibration plots demonstrate linear ranges from 0.1 to 500 ng mL−1 with correlation coefficients from 0.9908 to 0.9939. The limits of detection (LOD) were between 0.03 and 0.1 ng mL−1. To evaluate the repeatability, relative standard deviations (RSD) were evaluated for 0.1, 10, and 100 ng mL−1 of the aromatic amines, yielding values from 3.2% to 4.5%. The developed method was employed to extract aromatic amines from tap water, seawater, and spring water. The relative recoveries were from 97.2% to 99.9%. [ABSTRACT FROM AUTHOR]

Indacaterol, a β2 agonist prescribed for long-term management of patients with chronic obstructive pulmonary disease and asthma. In this study the first MISPE cartridges was developed using indacaterol as a template for its selective extraction from rat lung tissues, enabling precise pharmacokinetic evaluation at the drug's site of action. A molecular imprinting polymer was synthesized using indacaterol as a template, methacrylic acid as a functional monomer and ethylene glycol dimethacrylate as a cross-linker with a molar ratio (1: 4: 20). The polymer was characterized by a high binding capacity of 9840 ± 0.86 and high selectivity with an imprinting factor of 4.53 ± 0.12. The synthesized polymer was utilized as a sorbent in solid-phase extraction to purify and extract indacaterol from lung tissue matrix. The optimum molecularly imprinted solid-phase extraction (MISPE) conditions were 20.0 mg of molecular imprinting polymer and non-imprinting polymer, acetonitrile as the loading solvent, acetonitrile: water (20: 80; by volume) as the washing solvent, and methanol: acetic acid (90: 10; by volume) as the eluting solvent. A pharmacokinetic study was performed for indacaterol in rat lungs using the synthesized and optimized MISPE cartridge as a tool for sample purification. These parameters were determined in the lung tissues of rats emphasizing the local exposure of indacaterol to its target organ. The Cmax and Tmax were 51.020 ± 2.810 µg mL− 1 and 0.083 ± 0.001 h, respectively. The AUC 0−24 and AUC0 − inf were 175.920 ± 1.053 and 542.000 ± 5.245 µg h mL− 1, respectively. The elimination rate constant was 0.014 ± 0.00012 h− 1 and the half-life time was 48.510 ± 0.012 h. This study successfully developed and optimized MISPE cartridges using indacaterol as a template, enabling precise pharmacokinetic evaluation in rat lung tissues. The cartridges demonstrated high binding capacity and selectivity, providing crucial insights into the local exposure of indacaterol at its site of action. [ABSTRACT FROM AUTHOR]

Background: Natural compounds are essential targets in anticancer research due to the toxic effects of current chemotherapy and drug resistance. Methods: Saponin extraction from Alcea rosea L. was carried out using 20% methanol and liquid-liquid extraction coupled with the Solid phase extraction (SPE) approach. The saponin fraction was explored for its cytotoxic activity against Huh-7 and MDA-MB-231 cancer cell lines and a non-cancer cell line (HUVEC). The cytotoxic activity and oxidative stress were assessed using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) and 2,7 dichlorofluorescein diacetate dyes respectively. The apoptotic potential was investigated using DAPI and acridine orange-ethidium bromide dual staining. Result: The saponin fraction exhibited cytotoxic potential against the cell lines investigated. The IC50 values of the saponin fraction were 49.02, 300 and 325 µg\mL against Huh-7, MDA-MB-231 and HUVEC cell lines, respectively. The cytotoxicity for the extract was dose-dependent. The saponin fraction calculated selectivity index (SI) value indicated high selectivity towards Huh-7 cells (SI= 6.62) compared with normal HUVEC cells. Huh-7 cells treated with saponin fraction showed cellular and nuclear morphological changes, such as apoptotic body formation and chromatin condensation, as observed using light and fluorescent microscopy. However, further investigation is required to assess the the saponin fraction as a potential therapeutic agent. [ABSTRACT FROM AUTHOR]

Anthraquinones exhibit a significant group of natural and synthetic quinone derivatives because of their biological activities and industrial applications. Rhamnaceae is one of the families known to contain different kinds of anthraquinones. In this study, it was aimed to quantify rhein, emodin, chrysophanol and physcion in fruits of Rhamnus petiolaris Boiss. & Balansa belonging to Rhamnaceae by solid phase extraction and high performance liquid chromatography with ultraviolet detection. The anthraquinones were separated using a C18 analytical column. Gradient elution was performed using a mobile phase consisted of 0.1% o -phosphoric acid solution and methanol. Analytes were detected at 254 nm. Calibration curves were prepared in the range of 0.25–5.00 μg/mL for rhein, chrysophanol, physcion, 1.00–50.00 μg/mL for emodin. Limits of detection and quantification were between 0.07–0.11 and 0.20–0.34 μg/mL, respectively. Relative standard deviations were ≤ 5.78% in repeatability and intermediate precision studies. Accuracy was determined as relative mean error (8.17–12.06%). Extraction was achieved by maceration with acetone and ethanol, followed by hydrophilic–lipophilic balance solid phase extraction. Recoveries were between 96.2 and 109.6%. The developed and validated method was successfully performed to quantify rhein, emodin, chrysophanol and physcion in R. petiolaris fruit extracts. Only physcion was not detected above limit of detection. [ABSTRACT FROM AUTHOR]

An analytical method is presented for determining the uranium concentration in water samples via energy-dispersive X-ray fluorescence (EDXRF) spectrometry after solid-phase extraction. For the preconcentration procedure, the 1-(-2-thiazolylazo)-2-naphthol (TAN) reagent was used to complex the analyte in the samples. After the percolation of the sample and retention of the complex on a C18 disk, analysis was performed directly on the solid phase via EDXRF. The pH, sample flow rate, and sample volume were analyzed in terms of the uranium extraction. Using a sample volume of 110.0 mL buffered at pH 6.5 and a flow rate of 1.0 mL min−1, an enrichment factor (EF) of 645 was achieved, with a limit of detection of 1.5 μg L−1. The relative standard deviation (RSD, %), calculated from replications of the experiment under recommended conditions (n = 10; 20 μg L−1), was 10%. The results of the analyte addition and recovery tests varied between 98 and 117%. The accuracy of the method was verified via analysis of a water reference material, with no significant difference between the obtained values and the certified values (95% confidence level). The method was applied to groundwater, river water, and tap water samples collected in Caetité, Bahia, Brazil, and the results were compared with those obtained via inductively coupled plasma‒mass spectrometry (ICP‒MS). All the collected samples presented uranium concentrations below the acceptable maximum limit for drinking water samples. [ABSTRACT FROM AUTHOR]

Digital light processing (DLP) 3DP, commercial acrylate-based photocurable resins, and thermally expandable microspheres-incorporated flexible photocurable resins were employed to fabricate an SPE column with a thermally expanded monolithic foam for extracting Mn, Co, Ni, Cu, Zn, Cd, and Pb ions prior to the determination using inductively coupled plasma mass spectrometry. After optimization of the thermally activated foaming, the design and fabrication of the SPE column, and the automatic analytical system, the DLP 3D-printed SPE column with the thermally expanded monolithic foam extracted the metal ions with up to 14.8-fold enhancement (relative to that without incorporating the microspheres), with absolute extraction efficiencies all higher than 95.6%, and method detection limits in the range from 0.5 to 5.2 ng L–1. We validated the reliability and applicability of this method by determination of the metal ions in several reference materials (CASS-4, SLRS-5, 1643f, and Seronorm Trace Elements Urine L-2) and spiked seawater, river water, ground water, and human urine samples. The results illustrated that to incorporate the thermally expandable microspheres into the photocurable resins with a post-printing heating treatment enabled the DLP 3D-printed thermally expanded monolithic foam to substantially improve the extraction of the metal ions, thereby extending the applicability of SPE devices fabricated by vat photopolymerization 3DP techniques. [ABSTRACT FROM AUTHOR]

A functional material was developed with specific recognition properties for aflatoxins for pre-processing enrichment and separation in the detection of aflatoxins in Chinese herbal medicines. In the experiment, ethyl coumarin-3-carboxylate, which has a highly similar structure to the oxonaphthalene o-ketone of aflatoxin, was selected as a pseudo-template, zinc acrylate, neutral red derivative, and methacrylic acid, which have complementary functions, were selected as co-monomers to prepare a pseudo-template multifunctional monomer molecularly imprinted polymer (MIP). The MIP obtained under the optimal preparation conditions has a maximum adsorption capacity of 0.036 mg/mg and an imprinting factor of 3.67. The physical property evaluation of the polymers by Fourier infrared spectrometer, scanning electron microscopy, pore size analyzer, thermogravimetric analyzer, and diffuse reflectance spectroscopy showed that the MIP were successfully prepared and porous spherical-like particles were obtained. The synthesized polymer was used as a solid-phase extraction agent for the separation of aflatoxins from the extract of spina date seed. The linear range of the developed method was 10–1000 ng/mL, the limit of detection was 0.36 ng/mL, the limit of quantification was 1.19 ng/mL, and the recoveries of the extracts at the concentration level of 0.2 μg/mL were in the range 88.0–93.4%, with relative standard deviations (RSDs) of 1.97% (n). The results showed that the preparation of MIPs using ethyl coumarin-3-carboxylate as a template was simple, economical, and convenient. It is expected to become a promising functional material for the enrichment and separation aflatoxins from complex matrices. [ABSTRACT FROM AUTHOR]

The preparation of samples for instrumental analysis is the most essential and time-consuming stage of the entire analytical process; it also has the greatest impact on the analysis results. Concentrating the sample, changing its matrix, and removing interferents are often necessary. Techniques for preparing samples for analysis are constantly being developed and modified to meet new challenges, facilitate work, and enable the determination of analytes in the most comprehensive concentration range possible. This paper focuses on using metal-organic frameworks (MOFs) as sorbents in the most popular techniques for preparing liquid samples for analysis, based on liquid-solid extraction. An increase in interest in MOFs-type materials has been observed for about 20 years, mainly due to their sorption properties, resulting, among others, from the high specific surface area, tunable pore size, and the theoretically wide possibility of their modification. This paper presents certain advantages and disadvantages of the most popular sample preparation techniques based on liquid-solid extraction, the newest trends in the application of MOFs as sorbents in those techniques, and, most importantly, presents the reader with a summary, which a specific technique and MOF for the desired application. To make a tailor-made and well-informed choice as to the extraction technique. [ABSTRACT FROM AUTHOR]

Dispersive solid-phase extraction (dSPE) is a crucial step for multiresidue analysis used to remove matrix components from extracts. This purification prevents contamination of instrumental equipment and improves method selectivity, sensitivity, and reproducibility. Therefore, a clean-up step is recommended, but an over-purified extract can lead to analyte loss due to adsorption to the sorbent. This study provides a systematic comparison of the advantages and disadvantages of the well-established dSPE sorbents PSA, GCB, and C18 and the novel dSPE sorbents chitin, chitosan, multi-walled carbon nanotube (MWCNT), and Z-Sep® (zirconium-based sorbent). They were tested regarding their clean-up capacity by visual inspection, UV, and GC-MS measurements. The recovery rates of 98 analytes, including pesticides, active pharmaceutical ingredients, and emerging environmental pollutants with a broad range of physicochemical properties, were determined by GC-MS/MS. Experiments were performed with five different matrices, commonly used in food analysis (spinach, orange, avocado, salmon, and bovine liver). Overall, Z-Sep® was the best sorbent regarding clean-up capacity, reducing matrix components to the greatest extent with a median of 50% in UV and GC-MS measurements, while MWCNTs had the largest impact on analyte recovery, with 14 analytes showing recoveries below 70%. PSA showed the best performance overall. [ABSTRACT FROM AUTHOR]

Quinolone antibiotics (QNs) contamination in the aquatic environment is a global public health issue considering their resistance and mobility. In this study, a simple, efficient, and sensitive method was developed for the accurate quantification of fifteen QNs in water using automated disk-based solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). By utilizing a 3M SDB-XC disk to enrich QNs from a 1000 mL water sample, the detection limits were improved to 0.008–0.055 ng/L due to the satisfactory enrichment factors of 897−1136, but only requiring about 60 min per six samples. The linearity of the method ranged from 0.05 to 100 μg/L for the 15 QNs, with correlation coefficients of 0.9992–0.9999, and the recoveries were in the range of 81–114%, with relative standard deviations of 0.2–13.3% (n = 6). The developed method was applicable for the quantification of trace QNs at low ng/L levels in drinking and environmental waters. The results showed that no QNs were detected in tap water, while three and four QNs were detected in the river water of Zhoushan and the seawater of Daiquyang and Yueqing Bay, East China, respectively, with a total concentration of 1.600–8.511 ng/L and 1.651–16.421 ng/L, respectively. Among the detected QNs, ofloxacin (OFL) was the predominant compound in river water, while enrofloxacin (ENR) was predominant in seawater. The risk quotient (RQ) results revealed that QNs posed a low risk to crustaceans and fish, but a low-to-medium risk to algae, and OFL presented the main ecological risk factor in river water, while ENR and CIP in seawater. Overall, the proposed automated disk-based SPE–UPLC–MS/MS method is highly efficient and sensitive, making it suitable for routine analysis of QNs in drinking and environmental waters. [ABSTRACT FROM AUTHOR]

The fruit of the date tree (Phoenix dactylifera L.) is increasingly recognized for its nutritional and functional value. This exotic fruit shows variable composition, influenced by factors such as variety, ripening stage, and climatic conditions. In this context, this study aimed to investigate the nutritional profile and the bioactive components, including phenolic compounds and oligosaccharides, in different varieties of dates from Saudi Arabia collected at the Tamr ripening stage. The HPLC-ESI-MS analysis identified a total of 15 phenolic compounds, principally phenolic acids and flavonoids. Among the varieties tested, Safawi exhibited the highest phenolic concentration (1132 µg/100 g dw). To the best of our knowledge, the oligosaccharide composition is described for the first time among different varieties, with Sukari showing the highest concentration (3.37 g/100 g dw). Moreover, the antioxidant capacity (DPPH, ABTS, and FRAP assays) was assessed following a solid-phase extraction (SPE) clean-up to remove interferents, especially sugars. These results provide valuable insights into the health-promoting properties of date fruit as a functional food and provide a foundation for further research into their industrial applications as functional ingredients. [ABSTRACT FROM AUTHOR]

Rifaximin and rifampicin are good broad-spectrum antimicrobials. The irrational use of antimicrobial drugs in veterinary clinics could threaten public health and food safety. It is necessary to develop a reliable detection method of the residue for enhancing the rational supervision of the use of such drugs, reducing and slowing down the generation of bacterial resistance, and promoting animal food safety and human health. So, this study developed an LC-MS/MS method for the detection of rifaximin and rifampicin residues in animal-origin foods. The residual rifaximin and rifampicin of homogenized test materials were extracted with acetonitrile-dichloromethane solution or acetonitrile in the presence of anhydrous sodium sulfate and vitamin C, purified by dispersible solid phase extraction, determined by LC-MS/MS, and quantified by the internal standard method. The specificity, sensitivity, matrix effect, accuracy, and precision of the method were investigated in the edible tissues of cattle, swine, or chicken. In addition, the stability of the standard stock solution and the standard working solution was also investigated. The method was suitable for the muscle, liver, kidney, fat, milk, and eggs of cattle, swine, or chicken, as well as fish and shrimp. The specificity of the method was good, and the detection of the analytes was not affected by different matrices. Both the LOD and LOQ of the two analytes were 5 μg/kg and 10 μg/kg, respectively. The results of matrix effects in each tissue were in the range of 80–120%; there were no significant matrix effects. The average accuracy of rifaximin and rifampicin in different foodstuffs of animal origin was between 80% and 120%, and the method precision was below 20% (RSD). The proposed method showed good performance for determination, which could be employed for the extraction, purification, and detection of residual rifaximin and rifampicin in edible animal tissues. The pretreatment procedure of tissue samples was simple and feasible. The method was highly specific, stable, reliable, and with high sensitivity, accuracy, and precision, which met the requirements of quantitative detection of veterinary drug residues. [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]

This review provides an overview of the current trends and prospects of the extraction and separation analysis techniques for phenolic compounds in honey in 2012–2022 years. The classification, chemical structures, physicochemical, and bioactive properties of phenolic compounds in honey were comprehensively analyzed. The recent sample preparation techniques for extracting and separating the phenolic compounds from honey were discussed. The advantages and disadvantages of different extraction and separation analyses were also analyzed and compared. According to recent literatures, solid phase extraction and liquid-liquid extraction, two traditional sample preparation techniques, are still widely used for extracting phenolic compounds from honey samples. Various improved microscale extraction methods, such as solid phase microextraction and liquid-liquid microextraction, and sub-technologies can be applied considering the recovery rates, costs, solvent consumption, and environmental impacts. This review will provide insights into the extraction and separation analysis of phenolic compounds, and foster the development and utilization of active components in honey. [ABSTRACT FROM AUTHOR]

Many fatal intoxications have been reported in connection with the consumption of newer, highly potent synthetic cannabinoids. Yet, a possible postmortem redistribution (PMR) might complicate reliable interpretation of analytical results. Thus, it is necessary to investigate the PMR-potential of new synthetic cannabinoids. The pig model has already proven to be suitable for this purpose. Hence, the aim of this study was to study the PMR of the synthetic cannabinoid 5F-MDMB-P7AICA and its main metabolite 5F-MDMB-P7AICA-dimethylbutanoic acid (DBA). 5F-MDMB-P7AICA (200 µg/kg body weight) was administered by inhalation to anesthetized and ventilated pigs. At the end of the experiment, the animals were euthanized and stored at room temperature for 3 days. Tissue and body fluid samples were taken daily. Specimens were analyzed after solid phase extraction using a standard addition method and LC–MS/MS, blood was quantified after protein precipitation using a validated method. In perimortem samples, 5F-MDMB-P7AICA was found mainly in adipose tissue, bile fluid, and duodenum contents. Small amounts of 5F-MDMB-P7AICA were found in blood, muscle, brain, liver, and lung. High concentrations of DBA were found primarily in bile fluid, duodenum contents, urine, and kidney/perirenal fat tissue. In the remaining tissues, rather low amounts could be found. In comparison to older synthetic cannabinoids, PMR of 5F-MDMB-P7AICA was less pronounced. Concentrations in blood also appear to remain relatively stable at a low level postmortem. Muscle, kidney, fat, and duodenum content are suitable alternative matrices for the detection of 5F-MDMB-P7AICA and DBA, if blood specimens are not available. In conclusion, concentrations of 5F-MDMB-P7AICA and its main metabolite DBA are not relevantly affected by PMR. [ABSTRACT FROM AUTHOR]

In this study, ultrasound-assisted dispersive magnetic solid phase extraction using toner powder (inexpensive and accessible magnetic sorbent) combined with flame atomic absorption spectrophotometry has been developed for the analysis of cobalt (II) in water and food samples. The influence of parameters (amount of toner powder, sample pH, the concentration of the complexing agent, eluent type and volume, and adsorption time) were studied as a function of the extraction recovery. The proposed method, which has been analytically characterized under its optimum operating conditions, allows the detection of cobalt (II) in the samples with method detection limits of 0.7 μg L−1. The method repeatability, expressed as the relative standard deviation (n = 10, Co2+= 50.0 μg L−1), was 3.1%, while the preconcentration factor was 50. Cobalt(II) was determined in water samples (tap water, river water, mineral water, seawater) and food samples (cabbage and cucumber) with good recoveries (96.0–104.0%) using the proposed method. [ABSTRACT FROM AUTHOR]

Copyright of Journal of Food Safety & Quality is the property of Journal of Food Safety & Quality 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.)

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.)