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A simple, rapid, and sensitive procedure is developed for the determination of hydroxylated polycyclic aromatic hydrocarbons (2-hydroxynaphthalene, 2-hydroxyfluorene, 9-hydroxyphenanthrene, 3-hydroxyphenanthrene, 2-hydroxyphenanthrene, 1-hydroxypyrene, and 6-hydroxychrysene) in urine by gas chromatography–mass spectrometry. Sample preparation is based on dispersive liquid–liquid microextraction with trichloromethane in an acidic medium. Derivatization is carried out in a heated injector port using the reagent N,O-bistrimethylsilyltrifluoroacetamide. The type of dispersing solvent is experimentally selected and the optimal ratio of the following factors, i.e., pH value, volume of dispersing solvent, and extraction time, is found using a three-factor experiment. A high-temperature capillary column NT-8 is used in a temperature gradient mode for analysis by gas chromatography–mass spectrometry. The linearity range of the calibration function is found to be 0.5–100 ng/mL. The developed procedure for determining hydroxylated PAH in urine is tested on urine samples from aluminum production workers. [ABSTRACT FROM AUTHOR]

A brief overview of chromatographic methods for determining free bisphenol A (BPA) in technical and food products is presented. Bisphenol A is used as a monomer in the production of some plastics and epoxy resins. The concentration of free BPA may exceed the permissible level in food plastic containers and in food products packaged in these containers. The maximum permissible concentration of BPA in water, in water bodies of domestic and drinking water and in cultural and household water use is 0.1 mg/dm3. In European countries, the migration value of BPA for plastics in contact with food products is 0.6 mg/kg. Gas chromatography with preliminary derivatization by the silylation or acylation of the analyte is most often used to determine BPA in plastics, food products, and biological fluids. Direct determination methods have been developed using gas-liquid chromatography on heat-resistant columns. Flame ionization, fluorometric, and mass-selective detectors are used as detection devices. HPLC with optical and mass-selective detectors is used to determine BPA. Thin-layer chromatography has also been used for determining BPA. Solid-phase extraction, liquid−liquid extraction, dispersive liquid−liquid microextraction, and a combined extraction method with separation in acetonitrile (QuEChERS) are used in BPA sample preparation. [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]

The room temperature ionic liquid trihexyl(tetradecyl)phosphonium decanoate ([P66614][Dec]) was employed in the liquid-liquid extraction of Co(II) from hydrochloric acid solutions in the presence of Ni(II). The extraction performance in liquid-liquid separations showed a strong dependence on the acid content of the feed aqueous solution. The best performance in terms of extracted cobalt and selectivity was obtained when the feed contained a HCl concentration above 6 M On the contrary, when the experiment was performed in absence of HCl, a lower extraction and Co/Ni selectivity were obtained. This behavior has been rationalized by considering the protonation of the [Dec]− anion and the different Co(II)/Ni(II) speciation in HCl media. Moreover, polymer inclusion membranes (PIMs) were prepared using PVC and [P66614][Dec] at different weight rations. Only the PIM formulated with a 30:70/PVC:[P66614][Dec] weight ratio demonstrated effective extraction of Co(II) from the HCl solution. The extraction efficiency and selectivity of the PIM was comparable to that from biphasic liquid experiments at 8 M HCl. The results of this study constitute a promising background for further practical developments of carboxylate-based ILs applied in Co/Ni separations. [ABSTRACT FROM AUTHOR]

This review article provides an overview of the fundamental background and application of aqueous two-phase systems (ATPSs) in protein and enzyme extraction. The types of ATPSs, including polymer/salt, polymer/polymer, alcohol/salt, surfactant-based, and ionic liquid-based ATPSs, are discussed, along with the unconventional ATPSs. Factors affecting partitioning in ATPSs, such as molecular weight and polymer concentration, pH, temperature, hydrophobicity, and affinity, are also examined. The article then focuses on the application of ATPSs in protein and enzyme extraction, including continuous processing and scaling-up. The future prospects, challenges, and limitations of ATPSs in this field are discussed, along with the challenges associated with their use in industry. The results section highlights the potential of citrate green salts as an alternative to sulfate and phosphate salts in salt-based ATPSs and the need for more research on using ionic liquids as an additive in ATPS types for protein and enzyme extraction. Overall, this review suggests combining cheap and environmentally friendly materials in ATPSs can be a practical solution for using ATPSs in the industry. [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.)

A novel Qingke Baijiu was produced by the process of light-aroma Baijiu combined with high-temperature stacking process and using highland barley of Tibet as material. Three kinds of Qingke Baijiu samples were evaluated by quantitative descriptive analysis, and analyzed by liquid-liquid extraction combined with gas chromatography-mass spectrometry and gas chromatography-olfactometry-mass spectrometry and analyzed by partial least squares regression analysis to clarify the aroma characteristic of the novel Qingke Baijiu and to investigate the influence of different manufacturing process. A total of 139 volatile compounds and 57 aroma compounds were detected in three samples, which included 11 aroma active compounds with odor active value (OAV) greater than 1. The total concentration of volatile compounds was 1.4 times higher after secondary fermentation. The sorghum and Zao aromas increased in the samples after secondary fermentation, where ethyl caprylate, ethyl caproate, ethyl isovalerate, and guaiacol were the corresponding key differential compounds. The sorghum and Zao aromas decreased after high-temperature stacking process, while floral aroma increased. Compared with the samples without high-temperature stacking process, the OAV of isoamyl acetate, guaiacol and 4-methylguaiacol increased, while the OAV of ethyl butyrate, ethyl caproate, and ethyl caprylate declined. After high-temperature stacking process, the concentration of isoamyl acetate increased, which lead to stronger floral aroma, and the concentration of butyric acid, ethyl caproate, ethyl caprylate, and ethyl decanoate declined, which lead to weaker sorghum aroma. [ABSTRACT FROM AUTHOR]

Solvent extraction of selenium(IV) ions from highly concentrated hydrochloric acid using 0.4 mol/L Aliquat 336 dissolved in kerosene was investigated. As a modifying agent, 1-octanol (10% v/v) was added to the organic phase to avoid the third phase formation. The effect of different parameters affecting the liquid-liquid extraction of selenium(IV) such as the acid concentration, shaking time, metal ion concentration in the aqueous phase, loading capacity, diluents, and temperature, was studied. The results indicate that selenium(IV) is extracted efficiently by 0.4 mol/L Aliquat 336 dissolved in kerosene. It was noticed that the extraction increased with the increase in the acid and Aliquat 336 concentrations, reaching an extraction percentage of about 92% at 8 mol/L HCl and 97.1% at 1 mol/L extractant. The extracted organic species is postulated to be [H2SeO2Cl2.2R4NCl]org by using the slope analysis method, and the value of Kex for selenium(IV) extraction was found to be 26.17 ± 2 M− 2. The structure of the extracted organic species was confirmed by FT-IR. The effect of diluents using various aliphatic and aromatic diluents indicated that kerosene is the most preferred diluent. This is owing to safety ground purpose, economic consideration, the lower cost, availability, and lower toxicity. Thermodynamic parameters indicate the endothermic nature for the solvent extraction of selenium(IV) for the investigated system according to the positive value obtained of the enthalpy change (ΔH). Depending on the obtained results, the method was used to recover selenium(IV) from a simulated solution synthesized in hydrochloric acid medium, which is expected in anode slime leach liquor solution. [ABSTRACT FROM AUTHOR]

Acrylamide is a hazardous chemical mainly synthesized during the thermal processing of foods representing a significant concern within the broader issue of food contaminants and their impact on public health. Acrylamide can be absorbed by the human body through dietary intake, respiration, dermal contact, and mucosa. The metabolic conversion of acrylamide into mercapturic acid metabolites and glycidamide results in several adverse and toxic effects. Therefore, this review explores the formation, toxicity, and metabolism of acrylamide. Hence, it is crucial to detect and ensure product quality via risk evaluation. Traditional analytical techniques for acrylamide detection often require expensive instrumentation and complex sample preparation, prompting the exploration of alternative, cost‐effective, sustainable methods. Here, we propose the utilization of carbon quantum dots (CQDs) synthesized through green approaches as a novel solution. CQDs display their immense potential for diverse applications due to their valuable properties such as biocompatibility, photocatalysis, and strong fluorescence. This review highlights the distinct potential of CQDs as a fluorescence probe for detecting acrylamide, showcasing their efficacy in addressing food safety concerns. In addition, various extraction and purification techniques for acrylamide such as QuEChERS, solid phase extraction, Carrez clarification, and dispersive liquid‐liquid microextraction are comprehensively reviewed. QuEChERS is regarded as a most promising technique for the extraction of acrylamide owing to its cost‐effective, rapid, and higher recovery rates. [ABSTRACT FROM AUTHOR]

A highly accurate, precise, and simple liquid chromatography-tandem mass spectrometry (LC–MS/MS) method for ketotifen (KTF) estimation from Beagle dog plasma was developed and validated, with ketotifen-d3 (KTF-d3) as the internal standard (IS). KTF and IS were detected on an API 4000 mass spectrometer in multiple reaction monitoring (MRM) mode in electrospray ionization (ESI) positive ionization mode. The transitions were monitored at m/z 310.2 → 96.0 for KTF and m/z 313.2 → 99.1 for IS. KTF and IS were extracted from plasma using liquid-liquid extraction with methyl tertiary-butyl ether and then analyzed for 3 min with extracted samples (7 µL) into the LC–MS/MS system. Analytes were separated on a Luna® Hilic column (50 × 2.0 mm i.d., 3 μm) using the Nexera X2 HPLC. The mobile phase A consisted of 10 mmol/L ammonium formate (pH 3.0), while mobile phase B consisted of 0.05% formic acid in acetonitrile. The ratio of mobile phase was 5:95 (v/v) at a flow rate of 0.2 mL/min. The method has been thoroughly validated in accordance with the bioanalytical method validation guidelines established by the Ministry of Food and Drug Safety in Korea and the U.S. Food and Drug Administration, addressing selectivity, lower limit of quantification, linearity, carryover, precision, accuracy, recovery, matrix effect, and stability. The developed LC–MS/MS method was effectively utilized for the bioequivalence assessment of ketotifen in Beagle dog plasma following the oral administration of ketotifen syrup. [ABSTRACT FROM AUTHOR]

Donepezil (DPZ), a piperidine-based reversible cholinesterase inhibitor, finds extensive use in treating Alzheimer's disease (AD). Originally designed as an oral formulation, DPZ encounters drawbacks such as a brief duration of action and reduced treatment effectiveness in elderly patients with memory impairment or difficulty swallowing medications. To address these issues and improve patient compliance, researchers are actively exploring alternative DPZ formulations. Consequently, reliable methods are necessary to quantitate DPZ in biological samples for in vivo assessment. Therefore, we propose an efficient, sensitive, wide-dynamic, and cost-effective method for quantitating DPZ in rat plasma. Our method employs liquid-liquid extraction (LLE) followed by liquid chromatography and tandem mass spectrometry, enabling in vivo evaluation of novel DPZ formulations. Notably, our method requires only 20 μL of rat plasma and employs icopezil as the internal standard—a cost-effective compound with chemical similarity to DPZ. We meticulously optimized LLE conditions, taking into account factor interactions through design of experiments (DOE). Our rapid and straightforward extraction and purification involved using 500 μL of pure methyl tert-butyl ether to extract DPZ from the sample within five minutes. The dynamic range of the method extends from 0.5 ng/mL to 1,000 ng/mL, demonstrating excellent sensitivity and suitability for pharmacokinetic studies across diverse DPZ formulations. Following the FDA guidelines, we rigorously validated the developed method, evaluating selectivity, linearity (with a coefficient of determination ≥0.9999), accuracy (ranging from 96.0% to 109.6%), precision (≤13.9%), matrix effect (92.2% to 103.8%), recovery (98.5% to 106.8%), the lower limit of quantitation (0.5 ng/mL), and stability. Finally, we effectively employed the validated method for the long-term pharmacokinetic assessment of a DPZ formulation. We expect that this approach will make a substantial contribution to the advancement of new DPZ formulations, ultimately benefiting individuals afflicted by AD. [ABSTRACT FROM AUTHOR]

The aim of this study was to investigate the extent of second-hand smoke exposure in younger population visiting nightclubs in Croatia by comparing the levels of nicotine and its main metabolites cotinine and trans-3′-hydroxycotinine (3HC) in urine samples taken from 22 participants before and after spending about three hours in a nightclub, stratified by smoking status (smokers and non-smokers). The samples were prepared by liquid-liquid extraction and analysed with gas chromatography-mass spectrometry. The presence of nicotine, cotinine, and 3HC was confirmed in all urine samples. Their median concentrations significantly differed between the two measurements in non-smokers. Our findings show that even a three-hour exposure to second-hand smoke can significantly increase the levels of nicotine and its metabolites in urine, which are indicative of exposure to other, harmful tobacco smoke substances. They also call for raising awareness of the health risks of exposure to second-hand smoke in the general population and among individuals who frequent nightclubs in particular. [ABSTRACT FROM AUTHOR]

Thorium is a radionuclide used in various environmental studies such as dating, sediment movement, soil–plant transfer studies, and contamination of waste from the natural fuel cycle. The liquid–liquid extraction method using tri-n-butyl phosphate (TBP) allows for the separation of Th from the accompanying actinides. However, the separation of Th and U present in the same sample is not trivial. This separation is influenced by the starting acid (HCl or HNO3), the concentration of TBP in an organic solvent, and the concentration of the acid used for re-extracting Th, which is typically HCl. Therefore, it is necessary to study these factors to ensure that the method has sufficient chemical yield and selectivity in complex matrices. This study presents a systematic investigation of the aforementioned parameters, making the necessary variations to select an optimal method for the radiochemical separation of Th. The ideal conditions were obtained using 4 M HCl as the acid prior to extraction, a 1:4 solution of TBP in xylene, and 4 M HCl as the re-extracting agent. The accuracy and precision were studied in four intercomparison exercises conducted in quadruplicate, using the parameters Enumbers, RB(%), and RSD(%) for 232Th and 230Th. The sensitivity of the method was experimentally studied and the limit of detection (LoD) was determined according to ISO 11929:2005. Additionally, the linearity of the method showed that the experimental and theoretical activity concentrations of 232Th and 230Th had slopes of 1 with an intercept close to 0. [ABSTRACT FROM AUTHOR]

The removal of nitrogen compounds from fuel via the conventional method, which is hydrodenitrogenation, is costly and involves catalysts and energy-intensive conditions (600 K and 300 atm). Recently, ionic liquids (ILs) have emerged as a promising alternative solvent for the denitrogenation of fuel oil. However, certain ILs are expensive and challenging to synthesize, prompting the exploration of protic ionic liquid (PIL) substitutes, which offer similar advantages to ILs. This study utilized the conductor-like screening model for real solvents (COSMO-RS) to predict the phase equilibria for three PILs—triethylammonium p-toluenesulfonate (TEA-TSA), triethylammonium salicylate (TEA-SA) and triethylammonium benzoate (TEA-BZ)—which were subsequently validated through experimental investigations. Liquid–liquid extraction experiments were conducted at 298 K and 1 atm, with pyrrole (serving as the model nitrogen compound) concentrations in n-hexadecane (representing the model fuel) ranging from 10 to 50 wt%. Additionally, the NRTL model effectively correlated the experimental tie lines. The obtained data indicated that TEA-TSA exhibited superior selectivity and distribution ratio compared to TEA-SA and TEA-BZ. All the ternary systems tested displayed positive slopes, suggesting a higher affinity of nitrogen compounds for the PIL. Supporting this observation, interaction energy (ΔE) and excess enthalpy (HE) were employed. The predicted outcomes revealed that TEA-TSA had high ΔE, and all PILs exhibited negative values of HE. The HE calculation underscored the significance of strong hydrogen bond interactions between pyrrole and the PIL for successful extraction. [ABSTRACT FROM AUTHOR]

A composite based on Fe3O4 nanoparticles, graphene oxide, and a ionic liquid (1-butyl-3-methylimidazolium-2-carboxylate) is proposed as a sorbent for the extraction of bisphenol A (BPA) from bottom sediments by matrix solid-phase dispersion (MSPD). The saturation magnetization of the synthesized sorbent is 34 emu/g. Grinding of bottom sediments and subsequent grinding with a sorbent was carried out in a ball mill. Some stages of MSPD were partially automated, in particular, the procedures of magnetic separation, BPA desorption, and sorbent regeneration. The recovery of BPA under the experimentally selected conditions (sorbent mass 0.5 g, time required to grind the sorbent 5 min) was 94%. The sorbent can withstand four sorption-desorption cycles without a loss of sorption capacity. To purify the matrix from interferents, washing with n-heptane was proposed. Bisphenol A was determined by gas chromatography–mass spectrometry after derivatization with acetic anhydride. The analytical characteristics of the method were established using model samples of bottom sediments artificially contaminated with BPA. The limit of determination using the developed method is 0.1 μg/kg, the linearity range of the calibration curve is 0.3–12 μg/kg (r2 = 0.994). As real samples for analysis, we used bottom sediments selected near the discharge of wastewater treatment plants in the city of Voronezh (Voronezh River and Don River). The BPA concentration in bottom sediments is 3.83–6.52 μg/kg. [ABSTRACT FROM AUTHOR]

Copyright of Farmacia is the property of Societatea de Stiinte Farmaceutice Romania 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.)

To investigate the distribution of flavor components in Luzhou-flavor base baijiu from different aged cellars, the aroma components in 18 samples of Luzhou-flavor base baijiu from three cellars of different ages were identified and quantified by direct injection (DI), liquid-liquid extraction (LLE) or vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction (VSLLME) combined with gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). The differences in flavor among different base baijiu samples was analyzed by chemometrics methods such as principal component analysis (PCA), partial least squares-discriminant analysis (PLS-DA), and Spearman’s correlation coefficient. The results suggested that 151, 154 and 159 volatile compounds were identified in base baijiu from freshly prepared cellar and those aged over 30 and 100 years. In total, 148 aroma compounds were common to the three base baijiu, accounting for 93.1% of the total number of identified compounds. The quantitative analysis of 61 major aroma compounds showed that the concentrations of ethyl caproate, ethyl butyrate, hexanoic acid, butyric acid and acetic acid in base baijiu from each cellar exceeded 100 mg/L. The concentration of ethyl caproate was the highest, ranging from 1 156.4 to 2 142.2 mg/L. Chemometric results indicated that the flavor similarity of base baijiu between the new and over-30-year-old cellars was higher when compared with the cellar aged over 100 years. This findings further strengthen the baijiu industry’s conventional knowledge of the influence of cellar age on the flavor of Luzhou-flavor baijiu.

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of nobiletin and tangeretin in rat plasma, and the plasma was processed by a simple liquid-liquid extraction method with ethyl acetate. The chromatographic column was UPLC HSS T3 (50 × 2.1 mm, 1.7 μm), the mobile phase was acetonitrile-water (containing 0.1% formic acid). Multiple reaction monitoring mode (MRM) was used for quantitative analysis, nobiletin m/z 403.29 → 373.14 (cone voltage 22v, collision voltage 28v), tangeretin m/z 373.28 → 343.17 (cone voltage 20v, collision voltage 28V), tangeretin m/z 373.28 → 343.17 (cone voltage 20V, collision voltage 28V) and internal standard vitexin m/z 433.14 → 313.03 (cone voltage 32v, collision voltage 26v). The pharmacokinetics of nobiletin and tangeretin were evaluated in rats. The established UPLC-MS/MS method in the range of 2–2,000 ng mL−1 was successfully applied to the pharmacokinetics, and the calculated bioavailability of nobiletin and tangeretin was 63.9 and 46.1%, respectively. [ABSTRACT FROM AUTHOR]

Abstract Artificial neural networks (ANNs) are biologically inspired algorithms designed to simulate the way in which the human brain processes information. In sample preparation for bioanalysis, liquid–liquid extraction (LLE) represents an important step with the extraction solvent selection is the key laborious step. In the current work, a robust and reliable ANNs model for LLE solvent prediction was generated which could predict the suitable solvent for analyte extraction. The developed ANNs model takes a set of chosen descriptors for the cited analyte as an input and predicts the corresponding Hansen solubility parameters of the suitable extraction solvent as a model output. Then, from the solvent combination’s appendix, the analyst can identify the proposed extraction solvents' combination for the cited analyte easily and efficiently. For the experimental validation of the model prediction capabilities, twenty structurally diverse drugs belonging to different pharmacological classes were extracted from human plasma. The extraction process was performed using the predicted extraction solvent combination for each drug and quantitively estimated by HPLC/UV methods to assess their extraction recovery. The developed LLE solvent prediction model is in- line with the global trend towards green chemistry since it limits the consumption of organic solvents.

Artificial neural networks (ANNs) are biologically inspired algorithms designed to simulate the way in which the human brain processes information. In sample preparation for bioanalysis, liquid–liquid extraction (LLE) represents an important step with the extraction solvent selection is the key laborious step. In the current work, a robust and reliable ANNs model for LLE solvent prediction was generated which could predict the suitable solvent for analyte extraction. The developed ANNs model takes a set of chosen descriptors for the cited analyte as an input and predicts the corresponding Hansen solubility parameters of the suitable extraction solvent as a model output. Then, from the solvent combination's appendix, the analyst can identify the proposed extraction solvents' combination for the cited analyte easily and efficiently. For the experimental validation of the model prediction capabilities, twenty structurally diverse drugs belonging to different pharmacological classes were extracted from human plasma. The extraction process was performed using the predicted extraction solvent combination for each drug and quantitively estimated by HPLC/UV methods to assess their extraction recovery. The developed LLE solvent prediction model is in- line with the global trend towards green chemistry since it limits the consumption of organic solvents. [ABSTRACT FROM AUTHOR]

Organophosphate flame retardants (OPFRs) are widely used as substitutes for traditional brominated flame retardants, necessitating a reliable and sensitive method for biomonitoring their urinary metabolites to assess human exposure. This study conducted biomonitoring of 10 metabolites of OPFRs in 152 adults and assessed their association with oxidative stress biomarkers 8-hydroxydeoxyguanosine and 8-hydroxyguanosine. Urinary metabolites of OPFRs were released via enzymatic deconjugation. The addition of sodium chloride to the urine samples increases the ionic strength, inducing a salting-out effect that reduces the solubility of these compounds, thereby facilitating their extraction with a mixture of ethyl acetate and acetonitrile. Then, the metabolites of OPFRs were quantified by ultra-high performance liquid chromatography-tandem mass spectrometry, and we validated the method for linear range, precision, matrix effect, and method detection limit. The detection limit of the metabolites of OPFRs ranged from 0.01 to 0.2 μg/L, and these metabolites were detected with high frequencies ranging from 25.0 to 98.68% in the urine samples. The concentration of bis (2-chloroethyl) phosphate was significantly higher in males than in females, with the geometric mean concentration of 0.88 μg/L for males and 0.53 μg/L for females, respectively. Spearman correlation analysis revealed weak but statistically significant positive correlations among the urinary metabolites. Bayesian kernel machine regression analysis showed a significant positive association between elevated urinary concentrations of metabolites of OPFRs and increased oxidative stress levels. Di-n-butyl phosphate was identified as the metabolite that significantly contributed to the elevated level of 8-hydroxyguanosine. [ABSTRACT FROM AUTHOR]

Kombucha is obtained by fermentation of tea and sugar by bacteria and yeast. This beverage has several beneficial effects, including antimicrobial activity. The objective of this study was to evaluate the antifungal activity of Kombucha extracts against dermatomycosiscausing fungi. Different types of Kombucha (black, white, green tea) and times of fermentation (10, 20, 30 days) were evaluated. Kombuchas were filtered, and extracts obtained by liquid-liquid extraction with ethyl acetate. Minimum inhibitory concentrations (MIC) were determined against clinical isolates of dermatophytes Trichophyton rubrum and T. mentagrophytes by broth microdilution. Toxicity tests and high-performance liquid chromatography (HPLC) were also performed. MIC ranged from 62.5-2000 µg/mL. Green tea Kombucha and 10-days fermentation extracts showed the best results. Toxicity was observed only for white tea Kombucha. Despite the chromatographic profiles, further studies are needed to characterize the active molecules. However, Kombucha extracts may constitute a viable alternative for new treatment strategies against dermatomycosis. [ABSTRACT FROM AUTHOR]

An ultra-performance liquid chromatography-tandem mass spectrometry method for estimating nitrofurantoin in K2EDTA human plasma has been developed using the liquid-liquid extraction technique. This method used electrospray ionization in negative mode for nitrofurantoin using triple quadruple mass spectrometry, with nitrofurantoin-13C3 employed as an internal standard. Nitrofurantoin was extracted via the liquid-liquid extraction method and separated on an analytical column Xbridge C18 (4.6 × 100 mm, 3.5 μm). Nitrofurantoin and nitrofurantoin-13C3 were performed using multiple-reaction monitoring acquisition modes with the transition of m/z from 237.06 to 152.05 (nitrofurantoin) and from 240.04 to 152.04 (nitrofurantoin-13C3). The linearity range for nitrofurantoin was optimized from 5 to 800 ng/mL, respectively. The average recovery of nitrofurantoin and nitrofurantoin-13C3 was 82.9 and 93.8%, respectively. The inter-precision ranged from 2.5 to 5.5%, and the inter-run accuracy range (deviation) ranged from –0.5 to 3.6% across quality control levels. The method was validated following USFDA guidelines and was determined to be straightforward, highly sensitive, precise, robust, and accurate. Therefore, it is suitable for routine quantification of nitrofurantoin in bulk drug and formulation. [ABSTRACT FROM AUTHOR]

A liquid–liquid extraction pretreatment method using n-hexane as the extractant was developed for the analysis of volatile aroma substances in three flavors (six cola samples, six lemon samples, and six orange samples) of carbonated beverages by gas chromatography–mass spectrometry (GC-MS). Quantitative analysis was conducted using the external standard method. The spiked recovery rate of α-terpineol was used as the evaluation criterion. Single-factor and response surface experiments were conducted to investigate the effects of extraction temperature, extraction time, and solvent-to-sample ratio. The results indicated that the maximum spiked recovery rate of α-terpineol, 81.00%, was achieved at an extraction temperature of 45 °C, extraction time of 30 min, and a solvent-to-sample ratio of 1 mL:15 mL. Thirty-four components were identified by GC-MS on the pretreated samples via the internal standard method. 1,4-Cineole, fenchyl alcohol, borneol, and α-terpineol are covered aroma substances in cola beverages. Two aromatic substances, D-limonene and α-terpineol, were detected in orange juices. α-Terpineol was detected in each lemon-flavor carbonated beverage sample. Going a step further, α-terpineol was detected in all 18 carbonated beverage samples and had high response values. The principal component analysis by functional group classification led to the conclusion that acids, phenols, hydrocarbons, alcohols, and ethers played a major contribution to the aroma of these 18 beverages. Increased separation of target compounds was found using the new pre-treatment methods, resulting in improved analytical resolution and selectivity. [ABSTRACT FROM AUTHOR]

The creation of conditions for the rational and multipurpose use of forests has become an urgent task within the forest industry. There is an active search for opportunities to use bio-oil derived from wood waste obtained through fast ablative pyrolysis. Bio-oil has a rich chemical composition, making it relevant to isolate individual chemical components from it. The main objective of this work was to investigate a method for extracting the phenolic fraction from the pyrolysis fluid of wood waste and to obtain and study samples of side fractions obtained during phenolic extraction. This paper describes a method for the fractionation of wood waste pyrolysis fluid based on a multi-stage complex process, including vacuum distillation, liquid-liquid extraction, and acidalkali precipitation. A detailed description and scheme of the processes are presented in the paper. The properties and chemical compositions of the obtained fractions were investigated. In the fractionation process, a phenolic fraction containing at least 60.38% of phenolic compounds was isolated. The first stage of the separation produces a fraction with a high content of acetic acid, while the third stage leads to the separation of a fraction containing sugars. Additionally, a fraction containing up to 22% furfural is formed. The fractions obtained at each separation step have both scientific and commercial potential, in addition to the target phenolic fraction. [ABSTRACT FROM AUTHOR]

Background: Q808 is a novel antiepileptic agent currently in development. In this study, we established and validated a LC-MS/MS method for the quantification of Q808 in Rhesus monkey plasma. Furthermore, we applied this method to investigate the pharmacokinetics of Q808 in Rhesus monkeys. Methods: Samples containing diazepam as an internal standard (IS) were subjected to liquid-liquid extraction (LLE) and separated using a Zorbax Extend C18 column. The detection of Q808 and IS was performed using multiple reaction monitoring mode (MRM), specifically monitoring precursor-to-product ion transitions at m/z 297.9 to 213.9 and m/z 285.2 to 193.1 for Q808 and IS, respectively. For the pharmacokinetic study of Q808, a total of 30 healthy Rhesus monkeys (half male and half female) were administered single oral doses, single IV doses, or multiple oral doses of Q808. Blood samples were collected at predetermined time points for subsequent pharmacokinetic analysis. Results: The developed LC-MS/MS method exhibited linearity within the concentration range of 1.5-750 ng/mL with intra-day precision ≤8.3% and inter-day precision ≤14.6%. Additionally, accuracy was found to be ≤3.4%. In the pharmacokinetic study involving single oral doses of Q808 in Rhesus monkeys, Q808 was absorbed with a median time to peak plasma concentration ranging from 4.50-6.00 h and was eliminated with a terminal elimination half-life (t1/2) between 9.34-11.31 h. No definitive conclusion regarding linear pharmacokinetic characteristics could be drawn. The absolute bioavailability was determined as 20.95%, indicating limited systemic exposure after oral administration. Multiple dosing did not result in significant accumulation based on an accumulation factor Rac value of 1.31. Conclusion: We have successfully developed and validated a rapid yet sensitive LC-MS/MS method for quantifying levels of Q808 in rhesus monkey plasma for the first time. The determination method and pharmacokinetic characteristics of Q808 in rhesus monkey support the next steps in drug development. [ABSTRACT FROM AUTHOR]

A novel ferrofluid prepared from a hydrophobic deep eutectic solvent (DES) and Fe3O4@graphite composite materials was introduced as a green microextraction medium for the separation and enrichment of trace estrogens in real samples. It was found that the ferrofluid greatly improved the capacity and selectivity of target analytes, benefiting from the enrichment of both DES and Fe3O4@graphite composite materials. Using a combination of high-performance liquid chromatography–fluorescence detection (HPLC-FLD) and vortex-assisted liquid–liquid microextraction (VALLME), a new method was established for simultaneous rapid processing and accurate determination of three estrogens (estradiol [E2], estriol [E3], and ethinyl estradiol [EE2]) in environmental water and urine samples. Key parameters affecting the extraction efficiency were optimized using a single-factor approach and response surface methodology. Under optimal conditions, this method yielded a low limit of detection (1.01 ng L−1, 3.03 ng L−1, and 25.0 ng L−1 for EE2, E2, and E3, respectively), wide linear range (3–200,000 ng L−1), high enrichment factors (9.81–47.2), and satisfactory recovery (73.8–129.0%). Compared with traditional analytical techniques, this method avoids the use of volatile toxic organic extraction solvents and cumbersome phase separation operations. [ABSTRACT FROM AUTHOR]

Introduction: The intersection between craft beer and the confectionery industry has become relevant due to the growing demand for food products with unique properties and nutritional benefits. Objective: To investigate and evaluate the potential of craft beer functional extracts as innovative ingredients in the production of confectionery products, considering both their organoleptic characteristics and potential nutritional benefits. Materials and Methods: Extractions of different types of craft beer were carried out using a liquid-liquid extraction process, followed by analyses to determine their chemical composition, bioactive compound profile and antioxidant capacities. In addition, applicability tests were performed on confectionery products to evaluate both the impact on sensory quality and added nutritional properties. Results and Discussion: The results demonstrated that functional craft beer extracts contain a variety of bioactive compounds, including phenols and other antioxidants, which improve sensory characteristics and provide potential health benefits due to these antioxidant properties. Conclusions: The integration of functional extracts from craft beer in the confectionery industry emerges as an innovative strategy, which allows sensory enrichment of various products and may also provide nutritional benefits. This approach represents an example of how collaborations between seemingly different sectors can generate novel and attractive solutions to meet changing consumer demands and improve food quality. [ABSTRACT FROM AUTHOR]

A novel chromogenic system for the liquid-liquid extraction and determination of trace amounts of tungsten(VI) was investigated. The system comprises 4-nitrocatechol (4NC) as a chromogenic reagent, sulfuric acid as a complexing medium, and benzalkonium chloride (BAC) as a source of bulky cations (BA+), which readily form chloroform-extractable ion-association complexes. The impact of foreign ions and reagents was studied, and the optimal conditions for the sensitive, selective, and inexpensive determination of tungsten(VI) were identified. The limit of detection, linear working range, and molar absorptivity at λmax (422 nm) were determined to be 31 ng cm-3, 0.1-4.4 µg cm-3, and 5.49 × 104 dm3 mol-1 cm-1, respectively. The composition of the extracted complex was 1:2:2 (W:4NC:BA). Two potential structures of its anionic component, [WO2(4NC)2]2-, were discussed based on optimizations at the B3LYP/CEP-4G theoretical level and comparison between theoretical and experimental spectra. [ABSTRACT FROM AUTHOR]

Photointiators have been commercially applied in ultra-violet photocuring ink, varnish, coating, lacquers since 1970s. The significant advantages of efficient, energy-saving and environmental-friendly make them more and more popular in automobile industry, package industry, etc. Photointiators can reach foodstuff by vapour or diffusion from the food contact layer of the package. Although UV ink is just printed in the outer surface of the package, the residue photointiators can transfer to the inner surface by “set-off” effect. Different photointiator has different chemical and physical properties, and shows different response by different testing instrument. In this study, two methods of liquid chromatography time-of-flight mass spectrometry (LC-QTOF MS) and gas chromatography triple quadrupole mass spectrometry (GC-MS/MS) were developed for determination of migration for 23 photoinitiators in food contact coating. The response of the photointiators by two methods was compared for method selection. For the LC-QTOF MS method, an Hypersil GOLD AQ C18 column was utilized and 0.1% formic acid water-methanol was used as mobile phase. QTOF MS was performed by electrospray ion source positive ion mode (ESI+ ) and mutiple reaction monitor high resolution (MRM HR) mode. Simple dilution with acidified methanol was used for migration solution pretreatment and internal standard method was used for quantification. The limits of detection are from 0.002 5 to 0.01 mg/kg. Recoveries range from 60.9% to 124%, and the relative standard deviations (RSDs) are between 0.9% and 11.6%. For GC-MS/MS method, a CD-5 column was used, and the MS/MS was operated under MRM mode. Liquid-liquid extraction with n-hexane was used for migration solution pretreatment and internal standard method was also used for quantification. The limits of detection range from 0.000 4 to 0.002 mg/kg. The recoveries range from 77.0% to 128%, with RSDs are between 0.4% and 8.1%. Migration solution of 13 batches of metal coating samples were tested, while 5 of them are positive of photoinitiaor TPO or 2,4-diethyl-9Hthioxanthen-9-one, while the maximum detection value of photoinitiaor TPO is 0.050 2 mg/kg, the detection values of 2,4-diethyl-9H-thioxanthen-9-one are all less than 0.002 mg/kg. The two methods are easy, sensitive and accuracy, which can determine the migration of photointiators in food contact coating. [ABSTRACT FROM AUTHOR]

Methyl acrylate has a wide range of uses, but the production process usually produces aqueous by-products. In this study, four commonly used alcohols (1-pentanol, 1-hexanol, 1-heptanol, and 1-octanol) were selected as extractants to explore the liquid–liquid extraction behavior of water + methyl acrylate + extractants. Through the analysis of partition coefficient (D) and separation coefficient (S), it is found that the data of all systems are greater than 1, indicating that all four alkyl alcohols can well separate methyl acrylate from aqueous solution, and 1-octanol is the best. In addition, the consistency between the binary interaction parameters of regression and tie-line data was tested using Matlab tools, proving that the obtained parameters have good consistency. [ABSTRACT FROM AUTHOR]

The dispersive liquid-liquid microextraction (DLLME) is one of the most popular miniaturized extraction procedures. In this paper, the degree of dispersion and dispersion stability were studied with the aim to assess the correlations of these parameters with efficiency for the selected analytical application. The dependence between the degree of dispersion (cloudy state quality) and its stability obtained by various emulsification procedures, such as solvent-assisted emulsification (using various dispersive solvents) and mechanical emulsification (using auxiliary energies), is investigated and discussed. It was found out that the degree of dispersion depends on the type of emulsification procedure and decreases in the series: solvent-assisted (SA-) = ultrasound-assisted (UA-) > air-assisted (AA-) > vortex-assisted (VA-) emulsification. The emulsion stability depends on the degree of dispersion and there were 1810 and 2070 s for the most effective emulsification procedures, such us solvent-assisted and ultrasound-assisted emulsification, respectively. A comparison between the sensitivity of the analytical methods (using spectrophotometric determination of the anionic surfactants) and the degree of dispersion have been made. The sensitivity of the methods was ranked as follows: DLLME > UA-LLME > VA-LLME > AA-LLME. [ABSTRACT FROM AUTHOR]

The utilization of supramolecular deep eutectic solvent eddy-assisted liquid–liquid microextraction utilizing 2-hydroxypropyl β-cyclodextrin (SUPRADES) has been identified as a successful method for pre-enriching Cu, Zn, and Mn in vegetable oil samples. Determination of each element was conducted by inductively coupled plasma optical emission spectrometry (ICP-OES) after digestion of metal-enriched phases. Various parameters were examined, including the composition of SUPRADES species [2HP-β-CD: DL-lactic acid], a cyclodextrin mass ratio of 20 wt%, a water bath temperature of 75 °C, an extractor volume of 800 μL, a dispersant volume of 50 μL, and an eddy current time of 5 min. Optimal conditions resulted in extraction rates of 99.6% for Cu, 105.2% for Zn, and 101.5% for Mn. The method exhibits a broad linear range spanning from 10 to 20,000 μg L−1, with determination coefficients exceeding 0.99 for all analytes. Enrichment coefficients of 24, 21, and 35 were observed. Limits of detection ranged from 0.89 to 1.30 μg L−1, while limits of quantification ranged from 3.23 to 4.29 μg L−1. The unique structural characteristics of the method enable the successful determination of trace elements in a variety of edible vegetable oils. [ABSTRACT FROM AUTHOR]

Allelopathy is a biological process in which one organism releases biochemicals that affect the growth and development of other organisms. The current investigation sought to determine the allelopathic effect of Rumex acetosella on white clover (Trifolium repens) growth and development by using its shoot extract (lower IC50 value) as a foliar treatment. Here, different concentrations (25, 50, 100, and 200 g/L) of shoot extract from Rumex acetosella were used as treatments. With increasing concentrations of shoot extract, the plant growth parameters, chlorophyll and total protein content of Trifolium repens decreased. On the other hand, ROS, such as O2.− and H2O2, and antioxidant enzymes, including SOD, CAT, and POD, increased with increasing shoot extract concentration. A phytohormonal study indicated that increased treatment concentrations increased ABA and SA levels while JA levels were reduced. For the identification of allelochemicals, liquid‒liquid extraction, thin-layer chromatography, and open-column chromatography were conducted using R. acetosella shoot extracts, followed by a seed bioassay on the separated layer. A lower IC50 value was obtained through GC/MS analysis. gammaSitosterol was identified as the most abundant component. The shoot extract of Rumex acetosella has strong allelochemical properties that may significantly impede the growth and development of Trifolium repens. This approach could help to understand the competitive abilities of this weed species and in further research provide an alternate weed management strategy. [ABSTRACT FROM AUTHOR]

Introduction: Systemic and local steroid hormone levels may function as novel prognostic and predictive biomarkers in breast cancer patients. We aimed at developing a novel liquid chromatography-tandem mass spectrometry (LC-MS/ MS) method for the simultaneous measurement of multiple, biologically pivotal steroid hormones in human serum and breast cancer tissue. Methods: The quantitative method consisted of liquid-liquid extraction, Sephadex LH-20 chromatography for tissue extracts, and analysis of steroid hormones by liquid-chromatography-tandem mass spectrometry. We analyzed serum and tissue steroid hormone levels in 16 and 40 breast cancer patients, respectively, and assessed their correlations with clinical parameters. Results: The method included quantification of nine steroid hormones in serum [including cortisol, cortisone, corticosterone, estrone (E1), 17b-estradiol (E2), 17a-hydroxyprogesterone, androstenedione (A4), testosterone and progesterone) and six (including cortisone, corticosterone, E1, E2, A4, and testosterone) in cancer tissue. The lower limits of quantification were between 0.003–10 ng/ml for serum (250 µl) and 0.038–125 pg/mg for tissue (20 mg), respectively. Accuracy was between 98%-126%, intra-assay coefficient of variations (CV) was below 15%, and inter-assay CV were below 11%. The analytical recoveries for tissue were between 76%-110%. Tissue levels of E1 were positively correlated with tissue E2 levels (p<0.001), and with serum levels of E1, E2 and A4 (p<0.01). Tissue E2 levels were positively associated with serum E1 levels (p=0.02), but not with serum E2 levels (p=0.12). The levels of tissue E2 and ratios of E1 to A4 levels (an index for aromatase activity) were significantly higher in patients with larger tumors (p=0.03 and p=0.02, respectively). Conclusions: The method was convenient and suitable for a specific and accurate profiling of clinically important steroid hormones in serum. However, the sensitivity of the profile method in steroid analysis in tissue samples is limited, but it can be used for the analysis of steroids in breast cancer tissues if the size of the sample or its steroid content is sufficient. [ABSTRACT FROM AUTHOR]

Citrus aurantium L. hydrosol extracted by steam distillation from its flowers is a highly consumed herbal product in the Iranian traditional market, widely used as a food flavour and therapeutic food and drinks. This study investigated ten commercial hydrosol samples of C. aurantium flowers produced by conventional industrial processes, as well as a laboratory-prepared control sample. A liquid-liquid extraction method and sonication were used to extract essential oils from commercial hydrosols. Samples were then subjected to GC/MS analysis. ATR-IR spectroscopy was another efficient tool used to analyze hydrosol samples. All HPTLC chromatograms exhibited a close resemblance between samples and controls. The cluster analysis was used to compare the results of GC/MS and IR screening. In the HCA dendrograms derived from the GC/MS data, most of the oil sample profiles were found to be very similar to those of the control. Linalool was the most abundant compound in eight samples and the control. α-Terpineol in all hydrosol samples and geraniol in control and five other samples were the marker compounds. Ethyl disul- fide, dillapiol, and hotrienol were detected in two samples that have not been reported in previous studies and might have resulted from the addition of other herbal hydrosols. Microbial content and pH values were within permissible limits in all samples, making them safe for oral consumption. [ABSTRACT FROM AUTHOR]

Three ionic liquids (ILs) and three deep eutectic solvents (DESs) with identical counterparts, as well as their aqueous solutions, were prepared for the selective extraction of alginate from Sargassum tenerrimum, a brown seaweed. It was found that the ILs and their hydrated systems were only able to extract alginate from the seaweed directly, while the DESs were not, as confirmed by molecular docking studies. When the quality of the polysaccharide was compared to that produced using the hydrated IL system with the widely used conventional method, it was discovered that the physicochemical and rheological characteristics of the alginate produced using the ILs as solvents were on par with those produced using the conventional method. The ILs can be seen as acceptable alternative solvents for the simple extraction of the polysaccharide straight from the seaweed given the consistency of the extraction procedure used in conventional extraction processes. The hydrated ILs were discovered to be more effective than their non-hydrated counterparts. The yield was also maximized up to 54%, which is much more than that obtained using a traditional approach. Moreover, the ionic liquids can also be recovered and reused for the extraction process. Additionally, any residual material remaining after the extraction process was converted into cellulose, making the process environmentally friendly and sustainable. [ABSTRACT FROM AUTHOR]

Oxygenated compounds such as acids in bio-oils (BO) have been related to the corrosion of metals and their storage instability when applied as fuels. Therefore, upgrading BO by removing acids (deacidification) can be a valuable technique to reduce corrosivity using specific separation processes. Therefore, the objective of this paper was to evaluate the effect of the water content in the solvent (aqueous methanol), the carboxylic acid content in the BO and extraction temperature on the deacidification process by liquid–liquid extraction (LLE), as well as the effect of the same parameters on the quality of the deacidified BO through physical–chemical and GC-MS analyses. The results show that an increase in the water content (5 to 25%) in the solvent and an increase in the carboxylic acids content (24.38 to 51.56 mg KOH/g) in the BO reduce the solvent's capacity to extract carboxylic acids while increasing the temperature (25 to 35 °C) of the deacidification process promoted an increase in its capacity to remove them. Consequently, the highest deacidification efficiency (72.65%) is achieved with 5% water in methanol at 25 °C for BO1 (TAN = 24.38 mg KOH/g). Therefore, the deacidification process through LLE using aqueous methanol contributed significantly to BO upgrading. [ABSTRACT FROM AUTHOR]

Centrifugal contactors (CCs) are a technology candidate for the development of advanced reprocessing flowsheets. While they offer many advantages, such as process intensification, there are still uncertainties regarding their industrial deployment. The presence of particles in the process streams in particular may present a challenge to both performance and operability. Preliminary studies have been undertaken to evaluate the accumulation of particles in the contactors and the effect upon the extraction behaviour of nitric acid. Aluminium oxide (Al2O3) particles were suspended in the aqueous feed solution during the operation of a three-stage, 40 mm diameter CC cascade. The presence of insoluble solid particles in the aqueous feed, up to 7 g/L, were not observed to affect phase separation and entrainment under the experimental conditions investigated. The particles were centrifuged out of solution and accumulated as a thin cake/bed in the rotors of each stage. This work also illustrates that particles do entrain through the cascade. The predominant effect on the rate of accumulation was particle concentration in the aqueous feed solution, and increasing solids loading was observed to have an impact upon the extraction of nitric acid across the cascade. [ABSTRACT FROM AUTHOR]

Plants serve as reservoirs of bioactive compounds endowed by nature, rendering them promising subjects for investigating chemical diversity. Despite their potential, much remains untapped, whether in standardized extracts or isolated pure compounds. This unexplored terrain has paved the way for significant discoveries in pharmaceuticals. Notably, research has delved into the medicinal properties of Mallotus philippensis, a prominent plant in South Asia. Employing meticulous extraction techniques such as maceration, the fruit of this plant underwent initial antimicrobial screening, revealing encouraging results. Subsequent fractionation of the plant's extracts via liquid–liquid extractions, utilizing dichloromethane and absolute ethanol, facilitated further analysis. Evaluating these fractions for antibacterial activity demonstrated efficacy against various pathogenic microorganisms, particularly Pseudomonas aeruginosa and Escherichia coli, notably by the ethanolic and dichloromethane extracts. Furthermore, a comprehensive phytochemical analysis unveiled the presence of alkaloids, flavonoids, saponins, glycosides, phenols, and tannins. An assessment of the extracts' antioxidant potential via the 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging assay showcased significant activity, with a radical scavenging rate of 97%. This underscores the significance of utilizing fruit remnants, which are often rich in valuable chemical constituents yet commonly discarded, thereby adding value to both the species and the environment. Further investigation focused on the composition of Mallotus philippensis fruit, encompassing volatile and non-volatile metabolites through HPLC-MS analysis. Additionally, this study introduced the application of ionic liquid-loaded polysulfone microcapsules to enrich target constituents from crude extracts. An exploration of the key separation conditions, results, and recycling performance of these microcapsules provided insights for future research endeavors. Overall, this comprehensive study of Mallotus philippensis fruit extracts establishes a foundation for the ongoing exploration and development of this medicinal plant. [ABSTRACT FROM AUTHOR]

Indoxyl sulfate (IxS) and p-cresyl sulfate (pCS) are toxic uremic compounds with documented pathological outcomes. This review critically and comprehensively analyzes the available liquid chromatography-mass spectrometry methods quantifying IxS and pCS in human matrices and the biological applications of these validated assays. Embase, Medline, PubMed, Scopus, and Web of Science were searched until December 2023 to identify assays with complete analytical and validation data (N = 23). Subsequently, citation analysis with PubMed and Scopus was utilized to identify the biological applications for these assays (N = 45). The extraction methods, mobile phase compositions, chromatography, and ionization methods were evaluated with respect to overall assay performance (e.g., sensitivity, separation, interference). Most of the assays focused on human serum/plasma, utilizing acetonitrile or methanol (with ammonium acetate/formate or formic/acetic acid), liquid–liquid extraction, reverse phase (e.g., C18) chromatography, and gradient elution for analyte separation. Mass spectrometry conditions were also consistent in the identified papers, with negative electrospray ionization, select multiple reaction monitoring transitions and deuterated internal standards being the most common approaches. The validated biological applications indicated IxS and/or pCS were correlated with renal disease progression and cardiovascular outcomes, with limited data on central nervous system disorders. Methods for reducing IxS and/or pCS concentrations were also identified (e.g., drugs, natural products, diet, dialysis, transplantation) where inconsistent findings have been reported. The clinical monitoring of IxS and pCS is gaining significant interest, and this review will serve as a useful compendium for scientists and clinicians. [ABSTRACT FROM AUTHOR]

Thiosulfate leaching has been regarded as a promising alternative to cyanidation, but it still faces the challenge of the recovery of low content of gold from high concentrations of thiosulfate solutions. Liquid–liquid extraction is a method to address this issue but is still limited by the use of volatile and toxic organic solvents. To overcome this limitation, this work synthesized some functionalized dicationic ionic liquids (DILs) to serve as extraction solvents for the recovery of the gold–thiosulfate complex, [Au(S2O3)2]3−, from thiosulfate solutions. Experimental results indicated that the DILs showed higher extraction rates toward [Au(S2O3)2]3− compared with their monocationic-based counterparts, likely due to the stronger electrostatic interaction between the dications of the ILs and [Au(S2O3)2]3−. The transfer of [Au(S2O3)2]3− from the water phase to the IL phase was identified as an anion exchange and endothermic process. The rate of extraction was limited by the anion exchange process occurring at the IL–water interface. The extraction ability of ILs highly depended on the type of anion; specifically, the ILs with anions that had strong hydrogen-bonding ability exhibited high extraction ability toward [Au(S2O3)2]3−. Finally, DILs proved effective in the recovery of [Au(S2O3)2]3− from an actual gold leaching solution and exhibited high selectivity toward coexisting ions, indicating their potential as environmentally friendly solvents for gold recovery. [ABSTRACT FROM AUTHOR]

Beer is a popular alcoholic beverage worldwide. However, limited research has been conducted on identifying key odor-active components in lager-type draft beers for the Chinese market. Therefore, this study aims to elucidate the odor characteristics of the four most popular draft beer brands through a sensory evaluation and an electronic nose. Subsequently, the four draft beers were analyzed through solid-phase microextraction and liquid–liquid extraction using a two-dimensional comprehensive gas chromatography–olfactometry–mass spectrometry analysis (GC×GC–O–MS). Fifty-five volatile odor compounds were detected through GC×GC–O–MS. Through an Aroma Extract Dilution Analysis, 22 key odor-active compounds with flavor dilution factors ≥ 16 were identified, with 11 compounds having odor activity values > one. An electronic nose analysis revealed significant disparities in the odor characteristics of the four samples, enabling their distinct identification. These findings help us to better understand the flavor characteristics of draft beer and the stylistic differences between different brands of products and provide a theoretical basis for objectively evaluating the quality differences between different brands of draft beer. [ABSTRACT FROM AUTHOR]

Membrane technology allows the separation of active compounds, providing an alternative to conventional methods such as column chromatography, liquid–liquid extraction, and solid–liquid extraction. The nanofiltration of a Muérdago (Tristerix tetrandus Mart.) fruit juice was realized to recover valuable metabolites using three different membranes (DL, NFW, and NDX (molecular weight cut-offs (MWCOs): 150~300, 300~500, and 500~700 Da, respectively)). The metabolites were identified by ESI-MS/MS. The results showed that the target compounds were effectively fractionated according to their different molecular weights (MWs). The tested membranes showed retention percentages (RPs) of up to 100% for several phenolics. However, lower RPs appeared in the case of coumaric acid (84.51 ± 6.43% (DL), 2.64 ± 2.21% (NFW), 51.95 ± 1.23% (NDX)) and some other phenolics. The RPs observed for the phenolics cryptochlorogenic acid and chlorogenic acid were 99.74 ± 0.21 and 99.91 ± 0.01% (DL membrane), 96.85 ± 0.83 and 99.20 ± 0.05% (NFW membrane), and 92.98 ± 2.34 and 98.65 ± 0.00% (NDX membrane), respectively. The phenolic quantification was realized by UHPLC-ESI-MS/MS. The DL membrane allowed the permeation of amino acids with the MW range of about 300~100 Da (aspartic acid, proline, tryptophan). This membrane allowed the highest permeate flux (22.10–27.73 L/m2h), followed by the membranes NDX (16.44–20.82 L/m2h) and NFW (12.40–14.45 L/m2h). Moreover, the DL membrane allowed the highest recovery of total compounds in the permeate during the concentration process (19.33%), followed by the membranes NFW (16.28%) and NDX (14.02%). Permeate fractions containing phenolics and amino acids were identified in the membrane permeates DL (10 metabolites identified), NFW (13 metabolites identified), and NDX (10 metabolites identified). Particularly, tryptophan was identified only in the DL permeate fractions obtained. Leucine and isoleucine were identified only in the NFW permeate fractions, whereas methionine and arginine were identified only in the NDX ones. Liquid permeates of great interest to the food and pharmaceutical industries were obtained from plant resources and are suitable for future process optimization and scale-up. [ABSTRACT FROM AUTHOR]

This study delves into the micro-occurrence states and enrichment mechanisms of residual oil, pivotal for advancing the production from tight sandstone reservoirs, particularly from the Chang 8 Member of the Upper Triassic Yanchang Formation, Ordos Basin. Through an analysis of 23 core samples, employing high-pressure mercury injection, field emission scanning electron microscopy, thin section, and X-ray diffraction techniques, distinct reservoir types were categorized. The utilization of environmental scanning electron microscope, multi-solvent continuous extraction, and an oil components separation system facilitated an intricate analysis of residual oil micro-occurrence states and their subsequent effects on porosity and permeability reduction across varying reservoir types. The findings accentuate the integral role of reservoir type in determining residual oil distribution within tight sandstone reservoirs. Favorable pore throat sorting and connectivity in specified reservoir types are identified as conducive to residual oil enrichment with a higher concentration of light components. In contrast, elevated carbonatite and clay content in other reservoir types leads to adsorption of heavy components, disrupting pore throat connectivity, and impeding crude oil filling. The varied interactions between oil and rock, oil–oil, and pore throat sealing significantly impact the distribution of oil components of residual oil, culminating in a notable reduction of porosity and permeability by 2.63% and 0.197 mD, with corresponding reduction rates of 27.19% and 46.69%, respectively. The insights derived from this study furnish a theoretical foundation for augmenting tight oil recovery and comprehending the enrichment mechanism of residual oil driven by the heterogeneity of tight sandstone reservoirs. [ABSTRACT FROM AUTHOR]

Separating hydroalcoholic mixtures remains a significant challenge in engineering. Liquid–liquid extraction has emerged as an appealing alternative method, because it avoids the need for the large energy inputs, volatile organic compounds, and high pressures that are typically required by other separation processes. This study explores the use of hydrophobic deep eutectic solvents (HDESs) composed of terpenes and 10-undecenoic acid as extraction agents for the liquid–liquid separation of hydroalcoholic mixtures composed of alcohols (ethanol, propan-1-ol, and propan-2-ol) and water. The water content in the solvents studied was notably low, reflecting their hydrophobic nature. For the dried HDES samples, the water content ranged from 553 to 4901 ppm. In contrast, the water-saturated samples exhibited higher water contents, ranging from 7250 to 20,864 ppm. The HDES based on thymol, DL-menthol, and L-menthol displayed a eutectic point at an xterpenes of approximately 0.67. These mixtures maintained a liquid state up to a mole fraction of terpenes around 0.75. In contrast, the HDES composed of carvacrol, fenchyl alcohol, and α-terpineol exhibited their eutectic point at an xterpenes near 0.5. Notably, these mixtures remained in a liquid state across the entire composition range studied. The 2:1 molar ratio (HBA:HBD) presented the best values for extracting alcohols, reaching 34.04%, 36.59%, and 39.78% for ethanol, propan-2-ol, and propan-1-ol, respectively. These results show that HDES can be applied to overcome issues with existing extraction solvents, increasing the separation efficiency and making the process eco-friendly. [ABSTRACT FROM AUTHOR]

The active ingredients in peppermint are widely used in the pharmaceutical, food, cosmetic, and other industries. The traditional methods for producing peppermint extract through hydrodistillation (HD) and percolation are long process with low efficiency. The aim of this study is the improvement of the extraction performance and the efficiency of the extract obtained from hot percolation via pulsed disk and doughnut columns (PDDC), which is one of the most important pieces of liquid–liquid extraction (LLE) equipment. Peppermint extract was used as the continuous phase in the PDDC. n‐Hexane was considered as the dispersed phase in this column. In this study, the effects of three operating parameters were investigated, including the pulse intensity, continuous phase height, and dispersed phase flow rate, on the extraction efficiency of active ingredients in peppermint. The response surface method (RSM) was used to investigate the effect of these parameters on the extraction efficiency. The efficiency of this column in the extracting of active ingredients from peppermint was measured by UV–vis spectrophotometry, via the absorption rate of the main active ingredients of peppermint (menthol) in the samples, and the efficiency was 75% on average. The experimental and theorical of dispersed phase mass transfer coefficient were evaluated and compared. The results showed that the PDDC improved the extraction and mass transfer. By increasing the flow rate of the dispersed phase and the height of the continuous phase, the extraction efficiency and the mass transfer coefficient were increased. [ABSTRACT FROM AUTHOR]

Process towers, whose purpose includes executing operations of mass transfer such as stripping, distillation, or liquid-liquid extraction, are usually constructed as vertical steel cylindrical pressurised shells, supported on a cylindrical skirt. Seismic risk analysts in an industrial setting, especially in NaTech context, are often faced with the issue that structural vulnerability models are not always available for the various industrial facilities. Process towers, although widespread, are one of those cases. The objective of the study presented in the paper is to simulate the behaviour of such towers when subjected to earthquake-induced ground shaking, with the goal of numerically deriving seismic fragility models. To this end, as a case study, two towers were considered with the same height and internal diameter, but different operating pressures, which determines the thickness of the pressure vessel and, consequently, the configuration of the anchorage system. For each of the two models, multi-stripe dynamic analysis was conducted, using a selection of hazard-consistent ground motion records, on joystick models. The results of the dynamic analyses are presented and their use for the derivation of fragility functions for certain damage states is discussed. This modelling strategy can contribute to streamline the fragility evaluation of such structures, given the variety of geometries which appear in industrial plants. [ABSTRACT FROM AUTHOR]

The production of nutraceuticals is a growing trend, as many consumers consider them an important part of the modern active lifestyle. Others rely on the use of nutraceuticals instead of prescribing pharmaceuticals to improve their health more naturally. One of the major concerns in the nutraceutical industry is the potential presence of contaminants. Even low concentrations of contaminant residues can be harmful, so analytical methods that are sensitive at ultratrace levels are needed. Dispersive liquid–liquid microextraction method combined with fast gas chromatography and mass spectrometry was developed for the inspection of pesticide residues in Carmelite drops. The most suitable recoveries are presented when the alcohol content is fixed at 20% in Carmelite drops. The method was validated; the linearity, limits of detection/quantification, the method accuracy and precision were obtained. The complex nutraceutical matrix causes significant complications in quantitative analysis; therefore, the main target of the work was placed on studying the effects of the matrix on the correct expression of the resulting concentration of contaminants in different types of samples. An in-depth study of matrix factors was carried out, and its relationship with the content of potential interferents from the medicinal products as well as other components added during the drops' production was discussed. Related medicinal plant-derived nutraceuticals were tested, the method was applied for real-life samples, and positive findings are herein reported. [ABSTRACT FROM AUTHOR]

Wine exerts a fundamental influence on the global market, and its aroma remains a crucial attribute contributing to its commercial value. The market could benefit significantly if a simple and cheap method of analyzing a wine's aromatic profile were developed. The purpose of this study is to develop such a method. A multi-analytical method for quantifying 39 volatile compounds of wine aroma was developed and validated using liquid–liquid extraction and gas chromatography/mass spectrometry/mass spectrometry (GC-MS/MS). The method was validated for its linearity, reproducibility, recovery, limit of detection, and limit of quantification and showed excellent results for almost all compounds. The method was applied to 25 commercial Protected Designation of Origin "Nemea" wines, and the results were compared and correlated with the sensory analysis results by a trained panel. The correlations among the parameters indicated that the newly developed GC-MS/MS method produces similar results to human responses. [ABSTRACT FROM AUTHOR]