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Aqueous two-phase systems (ATPS) can be described as an alternative to traditional liquid-liquid extraction systems, typically consisting of a polymer and a salt solution. An alternative polymer called polyvinylpyrrolidone (PVP) has emerged as a viable option for ATPS due to its low cost, stability, and potential. This study aimed to investigate the effect of the molecular weight of poly (vinylpyrrolidone) (PVP) (K17, K25, and K30) and the temperature (298.15, 303.15, and 308.15 K) in the system ATPSs composed of PVPs and sodium sulfate/potassium sulfate/tri sodium citrate. The tie-line data were determined by measuring the density (ρ) and refractive index (nD). Moreover, the phase compositions and plait point are investigated for different PVPs molecular weight, temperature, and salt type. In addition, the effect of these parameters on the binodal curve, tie-line length (TLL), and slope of tie line (STL) are analyzed in detail by comparing them with the literature data. The impact of the parameters on the binodal curves was investigated by utilizing the values of the effective excluded volume parameter (EEV) that were calculated from the LLE data. Furthermore, the binodal curves and the tie-line compositions were well-fitted by using some semi-empirical equations. The phase separation ability is enhanced with temperature and PVPs molecular weight. The modified UNIFAC-NRF is used to correlate the liquid-liquid equilibrium data of the studied systems and the optimized binary group interaction parameters were determined. [ABSTRACT FROM AUTHOR]

Depolymerization and subsequent capture of monomers is of interest for process efficiency and sustainability. Polyamide‐6 (PA‐6) can be depolymerized in aqueous solution using a homogeneous catalyst. To purify the ε‐caprolactam (CPL) monomer and recycle the catalyst, two potential crystallization‐based strategies are studied: direct crystallization from the reaction mixture and liquid‐liquid extraction prior to crystallization. Solubilities in water and promising organic solvents were measured and compared to predictions using perturbed‐chain statistical associating fluid theory (PC‐SAFT) or conductor‐like screening model for real solvents (COSMO‐RS). Detailed solid‐liquid equilibria (SLE) of the CPL/water system were investigated utilizing DSC and PXRD. This work provides an overview of important factors of PA‐6 depolymerization including recycling of tungstophosphoric acid (TPA) and purification of CPL monomers. A first conceptual process design to be further developed is derived. [ABSTRACT FROM AUTHOR]

AbstractMethaqualone, introduced in the 1960s as a sedative-hypnotic alternative to barbiturates, was withdrawn from the market due to its side effects and growing recreational use. Despite this, interest in methaqualone and its analogs remains high, raising concerns about potential abuse in the future.An ultra-high-performance liquid chromatography method coupled with triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS) was developed to determine nine methaqualone-related compounds simultaneously. Biological samples were prepared using liquid-liquid extraction with ethyl acetate at pH 9, quantification was performed in blood using multiple reaction monitoring (MRM) mode. Methaqualone-d7 served as an internal standard. The limit of quantification (LOQ) ranged from 0.1 to 0.2 ng/mL, with precision and accuracy within 20%. Recovery ranged from 84.2% to 113.7%.The developed method allowed chromatographic separation of all compounds tested, including two structural isomers: methtylmethaqualone and etaqualone. The mass spectra aquired from quadrupole time-of-flight mass spectrometer allowed for the elucidation of comprehensive fragmentation study of methaqualone derivatives.The described situation poses a significant problem from the analytical point of view, as well as interpretation and forensic toxicological expertise. The developed method will contribute to increased analytical capabilities and enhanced detection of compounds from the methaqualone group that may appear on the illicit market. [ABSTRACT FROM AUTHOR]

The complexity of the drug market and the constant updating of drugs have been challenging issues for drug regulatory authorities. With the emergence of new psychoactive substances (NPS) and the nonmedical use of prescription drugs, forensic and toxicology laboratories have had to adopt new drug screening methods and advanced instrumentation. Using high‐performance liquid chromatography coupled with Orbitrap mass spectrometry, we developed a screening method for common NPS and other drugs. Two milliliters of mixed solvent of n‐hexane and ethyl acetate (1:1, v:v) were added to 500 μL of blood or urine sample for liquid–liquid extraction, and methanol extraction was used for hair samples. The developed method was applied to 3897 samples (including 332 blood samples, 885 urine samples, and 2680 hair samples) taken from drug addicts in a province of China during 2019–2021. For urine and blood samples, the limits of detection (LODs) ranged from 1.68 pg/mL to 10.7 ng/mL. For hair samples, the LODs ranged from 3.30 × 10−5 to 4.21 × 10−3 ng/mg. The matrix effects of urine, blood, and hair samples were in the range of 47.6%–121%, 39.8%–139%, and 6.35%–118%, respectively. And the intra‐day precision was 3.5%–6.0% and the inter‐day precision was 4.18%–9.90%. Analysis of the actual samples showed an overall positive detection rate of 58.9%, with 5.32% of the samples indicating the use of multiple drugs. [ABSTRACT FROM AUTHOR]

This study aimed primarily to evaluate acrylamide (AA) concentration using rapid, simplified, cost-effective liquid-liquid extraction and gas chromatography-mass spectrometry (GC-MS) in the most common instant coffee products, and secondly, to calculate the health risk assessment of AA for adults and children. The acrylamide level was quantified using gas chromatography coupled with the mass spectrometry (GC-MS). The estimated daily intake (EDI), hazard quotient (HQ), and margin of exposure(MOE) was also calculated. According to the results, acrylamide levels in instant coffee were obtained between 0.5 to 440.9 μg/kg. The concentrations of acrylamide detected in all samples were below the recommended benchmark levels by the European Commission (<850 µg/kg). The overall mean was calculated 137.3 ± 25.7 for coffee mix powder samples and 154.8 ± 39.7 for pure powder samples. There was no significant difference in AA concentration between pure powder and coffee mix groups (P > 0.05). However, a significant difference in AA content was observed in different brands of pure powder as well as some groups of the coffee mix (P < 0.05). Furthermore, the health risk due to consumption of various type of coffee is negligible. [ABSTRACT FROM AUTHOR]

Ionic liquids (ILs) are promising solvents for separating aromatics from fuel oils. However, studies for separate polycyclic aromatics with ILs are rare and insufficient, and the impact of solute structure on extraction performance still needs to be determined. In this work, we use 1‐ethyl‐3‐methylimidazolium bis([trifluoromethyl]sulfonyl)imide ([EMIM][NTF2]) as an extractant to separate 1‐methylnaphthalene, quinoline, and benzothiophene from dodecane mixtures. Liquid–liquid equilibrium experiments identified the optimal operating conditions. Nine solute molecules, including five alkanes and four aromatic hydrocarbons, were used to study the relationship between extraction performance and solute structure. Molecular dynamics simulation and quantum chemistry calculations gave a deep insight and reasonable interpretation of the structure‐performance relationship at the molecular level. An industrial‐scale extraction process was proposed. The IL can be easily regenerated using heptane as a back‐extractive solvent. A high‐purity fuel oil with aromatic content below 0.5 wt% is obtained after 8‐stage extraction. [ABSTRACT FROM AUTHOR]

Algae are exclusively aquatic photosynthetic organisms that are microscopic or macroscopic, unicellular or multicellular and distributed across the globe. They are a potential source of food, feed, medicine and natural pigments. A variety of natural pigments are available from algae including chlorophyll a, b, c d, phycobiliproteins, carotenes and xanthophylls. The xanthophylls include acyloxyfucoxanthin, alloxanthin, astaxanthin, crocoxanthin, diadinoxanthin, diatoxanthin, fucoxanthin, loroxanthin, monadoxanthin, neoxanthin, nostoxanthin, perdinin, Prasinoxanthin, siphonaxanthin, vaucheriaxanthin, violaxanthin, lutein, zeaxanthin, β-cryptoxanthin, while carotenes include echinenone, α-carotene, β-carotene, γ-carotene, lycopene, phytoene, phytofluene. These pigments have applications as pharmaceuticals and nutraceuticals and in the food industry for beverages and animal feed production. The conventional methods for the extraction of pigments are solid-liquid extraction, liquid-liquid extraction and soxhlet extraction. All these methods are less efficient, time-consuming and have higher solvent consumption. For a standardized extraction of natural pigments from algal biomass advanced procedures are in practice which includes Supercritical fluid extraction, Pressurized liquid extraction, Microwave-assisted extraction, Pulsed electric field, Moderate electric field, Ultrahigh pressure extraction, Ultrasound-assisted extraction, Subcritical dimethyl ether extraction, Enzyme assisted extraction and Natural deep eutectic solvents. In the present review, these methods for pigment extraction from algae are discussed in detail. [ABSTRACT FROM AUTHOR]

AbstractResins impregnated with organic extractants regarded as effective adsorbent materials due to their ability for selective sorption. These resins consist of a polymeric material that is infused with accessible organic extractants. Furthermore, these resins merge the unique properties and the distinctive characteristics of both liquid-liquid extraction and solid-liquid sorption processes. In this work, the impregnation of Styrene divinyl benzene beads (SM-2 beads) with triisobutylphosphine sulfide (TIBPS = CYANEX 471X) was prepared. A SM-2 bead functionalized with CYANEX 471X (SM-2-TIBPS beads) was characterized using scanning electron microscope (SEM) and Fourier-transform infrared spectroscopy (FT-IR) techniques and investigated for recovery and separation of palladium ions from a 3 M nitric acid solution. Various parameters were studied, as shaking time effect, nitric acid concentration, SM-2-TIBPS beads weight, Pd(II) concentration and temperature. The Pd(II)/SM-2-TIBPS sorption system has an endothermic nature and was fitted with a Langmuir isotherm model with a 0.9860 regression factor. The kinetics modeling was fitted with PSO and IPD models with regression factors of 0.9889 and 0.9959, respectively. The maximum monolayer sorption capacity of SM-2-TIBPS was found to be 17.47 ± 0.9 mg/g. The sorption of Pd(II) from different media at 3 M takes the following sequence: HNO3 > HCl > H2SO4. Desorption of about 76.38 ± 2.4% was achieved with (1 M + 1 M) of thiourea + HCl after one desorption stage. Effect of other interfering ions, as Pt(II), Pb(II), Eu(III), Cu(II), Mo(VI), Co(III), Zr(IV), Fe(III), Cd(II), and Ce(III), indicates high separation factors between Pd(II) and other investigated metal ions, which ranged from 9.4 to 35. [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]

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]

Extracting and purifying lignin from wood without compromising cellulose quality is a challenging process. Lactic acid: choline chloride is a deep eutectic solvent (DES) that has been identified as acceptable delignification solvent, producing lignin and hemicellulose as byproducts to the cellulose. Hemicellulose is partly transformed into furanic compounds (such as furfural and 5-HMF). While the larger lignin can be obtained by water precipitation from DES, smaller lignin molecules and furanics can be recovered by liquid–liquid extraction (LLX), either directly or after precipitation of the larger lignin molecules. The presence of water in the DES after water precipitation reduced the mutual miscibility with the solvents, allowing the use of a wider range of solvents in the LLX process. In the precipitation step, all the larger molecular weight lignin (Mw > 5000 Da) can be recovered when adding at least 3.5:1 [g/g] water to DES-black liquor. For the LLX step, guaiacol was found as suitable alternative to the previously published 2-methyltetrahedrofuran (2-MTHF). In addition, here we report the use of 2,2,5,5-Tetramethyl oxolane (TMO), a recent addition to the palette of (potentially) bio-based solvents. The distribution coefficients of smaller lignin molecules and furanics in LLX with guaiacol, TMO and 2-MTHF were compared, revealing that smaller lignin molecules (500–5000 Da) can be recovered with a reasonable distribution coefficient by 2-MTHF and guaiacol. Furfural showed distribution coefficients of at least 1.27 in all three solvents. Guaiacol and TMO both showed a significantly lower lactic acid leaching than 2-MTHF. This makes them potential alternatives for 2-MTHF in this technique. [ABSTRACT FROM AUTHOR]

Aim & Objective: This study evaluates the potential of combining paclitaxel (PTX) and bortezomib (BTZ) for breast cancer therapy. Materials & Methods: The nanoformulation was optimized via Box-Behnken Design (BBD), with method validation adhering to US-FDA guidelines. Results: Multiple reaction monitoring transitions for PTX, BTZ and internal standard were m/z 855.80→286.60, 366.80→226.00 and 179.80→110.00, respectively. Elution done on C18 Luna column with 0.1% FA in MeOH:10 mM ammonium acetate. The size of nanoformulation was 133.9 ± 1.97 nm, PDI 0.19 ± 0.01 and zeta potential -19.20 ± 1.36 mV. Pharmacokinetics showed higher Cmax for PTX-BTZ-NE (313.75 ± 10.71 ng/ml PTX, 11.92 ± 0.53 ng/ml BTZ) versus free PTX-BTZ (104 ± 13.06 ng/ml PTX, 1.9 ± 0.08 ng/ml BTZ). Conclusion: Future findings will contribute to the treatment of breast cancer using PTX and BTZ. Graphical Abstract Article highlights The importance of paclitaxel (PTX) and bortezomib (BTZ) in combination with chemotherapy is demonstrated by recently published studies. An obstacle to measuring the results of translational research is the lack of an analytical or bioanalytical approach for simultaneously estimating PTX and BTZ. A gap in the scientific literature has been filled by the development and validation of an LC-MS/MS method for the co-estimation or simultaneous measurement of PTX and BTZ. Both moieties were resolved in a Phenomenex Luna (C18), (7.5 × 4.6 mm, 3μ) column with a 0.1% FA in MeOH:10 mM ammonium acetate, 80:20 (% v/v) mobile phase at 0.6 ml/min flow rate. According to the US-FDA, the developed method was validated in female Sprague–Dawley rats plasma for different characteristics, such as linearity, precision and accuracy, LLOQ and stability studies. The oral P.K profile of PTX and BTZ co-loaded in a nanoformulation has been investigated in young female Sprague–Dawley rats to support the applicability of the established LC-MS/MS methodology. With an LLOQ of 1.0 ng/ml for each drug and a run time of 6.0 min, the calibration curve was found linear for the 1–600 ng/ml concentration range. The proposed LC-MS/MS method was confirmed to be repeatable, precise and accurate. The developed LC-MS/MS method was successfully illustrated for the co-estimation or simultaneous estimation of both drugs in rat plasma to generate an oral P.K profile. US-FDA Guidance of Industry and Bioanalytical Method Validation criteria was followed for the co-estimation of PTX and BTZ and was applied to nanoformulation development and bioanalytical investigations. [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]

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 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]

Aromase™ H2 is an enzymatic cocktail marketed to intensify the aroma, promote clarity and overall flavor of tea by releasing aromatic compounds and antioxidants that are naturally glycosylated. The hydrolysis of a wide range of glycoconjugates is the key to its action, which can arise from the substrate promiscuity of the main diglycosidase or other enzymes that are in the mixture. The characterization focusing on the activity toward flavonoids at different pH values allowed to increase the cocktail ratio of diglycosidase to α-rhamnosidase activity. In that way, the free disaccharide rutinose was selectively obtained in a laboratory scale reactor with 90 % conversion after 3.5 h reaction at pH 8. Purification was carried out by liquid-liquid extraction, recovering the aglycone hesperetin. Subsequent extraction with activated carbon allowed a recovery of 84 % of the rutinose. This work demonstrates the practical application of a commercial cocktail for the selective hydrolysis of rutinosylated compounds. [Display omitted] • Aromase™ H2 activities were measured using flavonoids and synthetic substrates. • Selectivity of the hydrolysis was increased by modifying the reaction conditions. • Hesperidin was hydrolyzed at the heterosidic bond rendering rutinose. • Rutinose and hesperetin were produced in a laboratory scale reactor and purified. [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]

3D printed mixed matrix membrane (MMM) thin film, as a novel adsorbent, was introduced for the extraction of two steroid hormones from wastewater and tap water samples before their determination by high-performance liquid chromatography. The designed adsorbent was fabricated as thin film utilizing digital light processing (DLP) 3D printing. The thin film was made of acrylate photo resin, graphitic carbon nitride (g-C3N4), and polyvinylpyrrolidone and its application was investigated for thin film microextraction of 17β-estradiol (E2) and estrone (E1). The morphology of the 3D printed film surface and its chemical changes were studied using field emission scanning electron microscopy and attenuated total reflectance-Fourier transform infrared spectroscopy, respectively. The surface wettability of the proposed MMM films was measured by water contact angle analysis and its porosity was studied by N2 adsorption/desorption analysis. To attain optimal microextraction performance, optimization of both thin film composition and microextraction procedure was conducted, followed by a thorough evaluation of figures of merit under the optimized conditions. The limits of detection and quantitation were determined to be 1.5 and 5 µg L−1 for both E2 and E1. The linear dynamic range for both compounds was from 5 to 150 µg L−1. The method's repeatability was investigated on a single film for 6 extractions, as well as on 3 different films and the relative standard deviation values were 4.43 and 4.91 for E2 and 5.36 and 6.03 for E1, respectively. [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]

Magnetic ionic liquids (MILs) are a subclass of ionic liquids that exhibit paramagnetic properties intrinsically, without the need for additional magnetic particles. These properties can be attributed to the cations, anions, or both. Typically, MILs incorporate transition or inner‐transition metals within the anion structure. These adaptable liquids demonstrate remarkable physicochemical properties, notably a robust response to external magnetic fields. The body of research concerning the synthesis, characterization, and practical applications of MILs has expanded swiftly in recent times. This review delves into the latest research on the synthesis, properties, and utilization of MILs across various domains, including catalysis, fluid‐fluid separation, polymer science, and analytical chemistry. Within the realm of analytical chemistry, MILs are pivotal, serving as solvents in various analytical procedures such as dispersive liquid‐liquid micro‐extraction, matrix solid‐phase dispersion, and single‐drop micro‐extraction. Owing to their paramagnetic nature, MILs are instrumental in the separation process, streamlining organic reactions by obviating the need for traditional extraction or centrifugation steps. [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]

Deep eutectic solvents (DESs) composed of a beta-diketone and phosphine oxides featuring different alkyl chain lengths were prepared and then employed as liquid-liquid extraction and dissolution media for the separation of iron, cobalt, neodymium, and dysprosium. In the dissolution the more sterically hindered DESs exhibited enhanced selectivity to neodymium, which was poorly separated using liquid-liquid extraction. The dissolution selectivity in less sterically hindered DESs could be controlled by the addition of organic acids with different alkyl chain lengths. [ABSTRACT FROM AUTHOR]

In this work, we explored the impact of zwitterionic surfactants, sulfobetaine 16 (SB-16) and a PEG-phospholipid conjugate (DSPE-PEG), on nanosensor performance. We fabricated four sensors (for Na+, K+, Al3+, and O2) and examined how these surfactants influenced various aspects, including fabrication methods, sensing mechanisms, and the incorporation of nanomaterials. Our results highlighted SB-16's role in enhancing selectivity in ion-exchange sensors (Na+ and K+) while maintaining sensitivity akin to its PEG counterpart. The liquid–liquid extraction based sensors (Al3+) were unaffected by surfactant choice, while the O2 sensors that operate via collisional quenching exhibited reduced sensitivity with SB-16 when compared to its PEG-based counterpart. Additionally, the SB-16 sensors proved adaptable to different fabrication approaches (SESE – single emulsion solvent evaporation and FNP – flash nanoprecipitation), showcased good cell viability and maintained a functional lifetime of at least five days. Furthermore, via the use of quantum dots, we showed that it is possible to incorporate other nanomaterials into the sensing phase of SB-16 sensors. Future investigations could target enhancing the pH stability of zwitterionic surfactants to further advance their applicability in sensor technologies. [ABSTRACT FROM AUTHOR]

Efficient recognition and extraction of hazardous anionic pollutants from water medium is of great significance for environmental concerns, representing a challenging area of research in supramolecular chemistry. In this study, we present, for the first time, a comprehensive demonstration of the ability of chalcogen bonding (ChB) to recognize and remove the ReO4− from 100 % water medium. The anion recognition ability is well elucidated through solution phase NMR and ITC studies, which clearly reveal the selective binding of ReO4− over other oxo‐anions. Moreover, the selenoimidazolium scaffold effectively engages in Se•••O ChB interaction with ReO4− as confirmed by X‐ray crystal structure and XPS analysis. More importantly, the binding of ReO4− with different prolongations of the σ–holes, along with Se•••Se chalcogen bonding interactions, lead to the formation of a 1D supramolecular assembly. Eventually, ChB receptor Se4Me−Br exhibits ~62 % ReO4− extraction efficiency through precipitation as the extraction method. Furthermore, in efforts to enhance efficiency, a hydrophobic ChB receptor Se4Do‐PF6 has been prepared, achieving an efficiency of up to ~93 % at a very low concentration (~5 ppm) by liquid‐liquid extraction. [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]

A thermo‐assisted deep eutectic solvent (DES) based on dispersive liquid‐liquid microextraction followed by gas chromatography with flame ionization detection was developed for the analysis of five phthalate esters in different water samples. In the procedure involved, a DES composed of lidocaine, an amphiphilic amine, and oleic acid, was mixed with the sample assisted by ultrasound, and phase separation was achieved with increasing temperature. The heating of the extraction system induced the change of acid‐base properties of the DES components. Thus, the formation of microdroplets of DES in the sample was provided, and two phases were separated. The structure of the upper hydrophobic layer was characterized by Fourier‐transform infrared spectroscopy. Also, the amount of water in the DES phase was analyzed by mass spectrometer and Karl Fischer titration. Some critical variables on the extraction yield were assessed. The proposed method achieved 1.2–1.3 and 4.1–4.3 µg/L for limits of detection and limits of quantification, respectively. The intra‐day and inter‐day percentage relative standard deviations (n = 5) were determined to be in the range of 4.2–6.2% and 5.1–7.2%, respectively. Ultimately, this method analyzed the five phthalate esters in different water samples with high recoveries. [ABSTRACT FROM AUTHOR]

The separation and purification of bio-based chemicals from conversion processes often contribute substantially to bioprocessing costs, and for many biochemicals produced through fermentation, solventbased liquid--liquid extraction (LLE) is a common separations strategy for in situ product recovery (ISPR). Many in situ LLE-based separations for biochemicals are often challenged by emulsion formation between the immiscible aqueous and organic phases. Typically, membrane contactors have been used to overcome emulsion formation, with the aqueous and organic phases coming into contact in the membrane contactor pores, but these unit operations require a large membrane area to compensate for their limited effective interfacial area. In this study, we show that a hydrophobic polytetrafluoroethylene (PTFE) membrane-based emulsion separator (MBES) enables continuous LLE for the recovery of an exemplary fermentation product, butyric acid, with substantially improved throughput relative to a membrane contactor. With a membrane permeate flux of 290 L m-2 h-1, the overall butyric acid flux of the single-stage MBES system was calculated to be 1450 g m-2 h-1, which is substantially higher than the 9 g m-2 h-1 achievable with a membrane contactor. At an equivalent butyric acid throughput, process modeling estimates that MBES-assisted LLE can enable a 55% and 91% reduction in process costs (the sum of CAPEX and OPEX) and greenhouse gas emissions, respectively, compared to a membrane contactor due to a ~160-fold decrease in the required membrane area. Although membrane fouling from cellular debris led to reduced membrane flux and phase separation efficiency, common fouling mitigation strategies including the incorporation of ultrafiltration and periodic membrane backwashing effectively recovered the membrane performance. Overall, MBES systems can potentially enable continuous LLE processes in bioprocessing separations, including where emulsion formation is a challenge. [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]

A rapid and sensitive dispersive liquid–liquid microextraction (DLLME) method coupled with UV-Vis spectrophotometry has been developed and validated for the determination of metoclopramide in pharmaceutical and biological samples. The method is based on the formation of an ion-pair complex between metoclopramide and cobalt(II) thiocyanate under acidic conditions (pH = 3), followed by DLLME to efficiently preconcentrate the chromogenic complex. In the novel DLLME procedure, methylene chloride was used as the extraction solvent and acetonitrile acted as the dispersive solvent, generating a cloudy heterogeneous mixture upon injection into the aqueous sample. This facilitated extensive interfacial contact and partitioning of the metoclopramide-cobalt complex into the fine dispersed methylene chloride droplets within minutes. After centrifugation, the sedimented organic phase was analyzed at the maximum wavelength of 625 nm. Under optimal conditions, the method permitted quantification of metoclopramide from 0.25–45 µg/mL with high enrichment factors, and LOD of 0.078 µg/mL, LOQ of 0.258 µg/mL and high extraction recoveries in the range of 94–101% were obtained. The proposed DLLME-spectrophotometric methodology provides a simple, rapid and sensitive approach for routine therapeutic monitoring and quality control of metoclopramide in real samples. [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]

Safety and effectiveness are the two ends of the balance in drug development that needs to be evaluated. The biotransformation of drugs within a living organism could potentiate biochemical insults in the tissue and compromise the safety of drugs. Nitrofurantoin (NFT) is a cheap clinical antibiotic with a wide array of activities against gram-positive and gram-negative organisms. The NFT scaffold has been utilized to develop other derivates or analogues in the quest to repurpose drugs against other infectious diseases. Several techniques were developed over the years to study the mechanism of NFT metabolism and toxicity, such as voltammetry, chromatographic analysis, protein precipitation, liquid-liquid extraction, etc. Due to limitations in these methods, the mechanism of NFT biotransformation in the cell is poorly understood. Metabolomics has been adopted in drug metabolism to understand the mechanism of drug toxicity and could provide a solution to overcome the limitations of current techniques to determine mechanisms of toxicity. Unfortunately, little or no information regarding the metabolomics approach in NFT metabolism and toxicity is available. Hence, this review highlights the metabolomic techniques that can be adopted in NFT metabolism and toxicological studies to encourage the research community to widely adopt and utilize metabolomics in understanding NFT's metabolism and toxicity. [ABSTRACT FROM AUTHOR]

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

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

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This study aims to develop a liquid-liquid equilibrium model to predict the Ce distribution in the extraction system based on experimental laboratory data. Extraction feed solution (Ce hydroxide in nitric acid media) and solvent (Tri Butyl Phosphate (TBP) in kerosene diluent) with a volume ratio of 1:1 at various concentrations of feed and solvent were contacted using a mechanical shaker at 150 rpm for 15 minutes. The solution was settled for 30 minutes to separate the aqueous and organic phases. Cerium concentration in the aqueous phase was analyzed using XRF, while cerium concentration in the organic phase was calculated using a mass balance. The results showed that the extraction of Ce from the Ce-hydroxide concentrate was successfully carried out using TBP 0.92 M in kerosene diluent so that the Ce extraction efficiency of 70% was obtained. The equilibrium model that has been developed was able to represent the phenomenon of the liquid-liquid equilibrium distribution in the extraction system, which was carried out with an average relative error of 8.53%. Five stages of extraction unit need to apply to achieve 90% of extraction efficiency. [ABSTRACT FROM AUTHOR]

This study focuses on numerically optimizing key process parameters related to the liquid–liquid extraction batch process (LLEBP) technique for carrying out batch runs to remove methyl red effectively (MR) from dye effluent. LLEBP, a suitable industrial process for treating dye effluents, depends on the number of reaction parameters such as feed concentration, extraction time, and dye ratio (solution/solvent). The current research utilized a central composite design (CCD) of experiments along with numerical optimization techniques to optimize process parameters over a range of dye concentrations: (20–100) ppm, extraction time range 10–30 min, and dye ratio 1–3 mL/mL (solution/solvent). The batch runs performed at room temperature and a constant pH of 3, according to the experimental design criteria, suggest that maximum dye removal efficiency and distribution coefficient value could be achieved within the feed concentration range of (20–30) ppm, 20–30 min of extraction time, and 1–3 mL/mL of dye ratio (solution/solvent). Solvent capacity increases significantly within the (60–100) ppm feed concentration range. Numerical optimization with desirability function criteria identified optimal conditions: 20 ppm dye concentration, 30 min extraction time, and 3 mL/mL dye ratio ensuring maximum LLEBP yield. The current investigation achieved a 4% higher dye removal (%) of 85.682 compared to the previous study. The distribution coefficient and solvent capacity attained were 5.287 and 4.504 mg/L, respectively. The research enhances understanding of the optimization process for LLEBP in MR dye removal from textile effluent, surpassing previous findings within the same input range. The manuscript aims to maximize process optimization using CCD, promoting sustainable industry progress in line with UN sustainable development goals. [ABSTRACT FROM AUTHOR]

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.

In this study, a dispersive liquid–liquid microextraction along with a back-extraction step (DLLME-BE) has been developed for the determination of thre antidepressant drugs (citalopram, sertraline, and venlafaxine) in biological samples prior to HPLC-UV. Briefly, the method involved two main steps: first, a deep eutectic solvent (DES) composed of tetrabutylammonium bromide (TBABr as a dispersive agent) and 1-dodecanol (as the extraction solvent) was decomposed in an aqueous phase and led to in situ dispersion of the organic phase and extraction of analytes.. Second, Air-assisted liquid–liquid microextraction (AALLME) was applied to back-extract analytes into 50 µL of an aqueous acceptor phase while many interferences were not able to extract into the acceptor solution. By performing this developed extraction method, a high sample clean-up was achieved. The maximum efficiency of analytes was obtained based on the optimisation of the main parameters. Validation of the method indicated that the limits of detection (LODs) and limits of quantifications (LOQs) were in the range of 0.7–3.9 µg L−1 and 2.1–9.8 µg L−1 respectively. The extraction recoveries and enrichment factors of analytes were obtained to be in the range of 87.1–99.1% and 89–102, respectively. Finally, the method was utilised for extraction of three antidepressant drugs in water, human urine and plasma samples. [ABSTRACT FROM AUTHOR]

In this study, accurate and sensitive determination of ibuprofen in blood, urine, pharmaceutical tablet, syrup, and water samples was accomplished with the combination use of deep eutectic solvent-based ultrasound-assisted liquid–liquid microextraction (DES-UA-LLME) and high-performance liquid chromatography-ultraviolet visible detection system. The most important advantage of this method is that it can be used in the determination of ibuprofen without affecting the matrix environment of a wide range of samples. Ibuprofen in the sample phase was extracted to 500 µL of deep eutectic solvents phase (ChCl:Ph at 1:4 molar ratios) at pH 3.0. The influence of analytical parameters, such as pH of sample solution, the molar ratio of deep eutectic solvents components, tetrahydrofuran volume, and volume of DESs, were optimised in details. The preconcentration factor (PF), the detection limit (DL), intraday, and interday relative standard deviations (RSD, %) for the developed DES-UA-LLME/HPLC procedure were found as 30, 0.4 µg L−1, 1.74%, and 4.68%, respectively. The developed DES-UA-LLME was successfully used for the determination of ibuprofen in urine, blood, pharmaceutical tablet, syrup, and water samples. [ABSTRACT FROM AUTHOR]

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.

5‐Hydroxymethylfurfural (HMF) was transformed into 2,5‐diformylfuran (DFF) with nitric acid as the oxidant. The initial HMF content was as high as 12.5 wt %, and water was the sole solvent. This is an intensely exothermic reaction along with the emission of NO2 gas. A high DFF yield of 83.2 % was achieved if the oxidation ability of nitric acid matched with the requirement of target oxidation reaction while mismatched those of side reactions by regulating the initial concentration of nitric acid (59.5 wt %) and reaction temperature (50–60 °C). The oxidation reaction of HMF, overoxidation of HMF, and skeleton‐cracking reaction of FDCA preferred concentrated HNO3, hot HNO3, and concentrated or hot HNO3, respectively. After liquid‐liquid extraction, filtration, and column chromatography, light‐yellow DFF powders with purity of 92.1 wt % and isolated yield of 40.2 % were obtained and confirmed by NMR, FTIR, UV‐Vis, and elemental analysis. HMF was the dominant impurity due to its affinity to DFF. In addition, chromogenic substances were obtained as a byproduct, and they were potential pH indicators. These chromogenic substances had highly conjugated molecular structures, and they were generated via successive β‐protonation‐based ring‐opening reaction of HMF, aldol reaction, and dehydration reaction. [ABSTRACT FROM AUTHOR]

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]