Liquid Liquid Extraction Research Papers (original) (raw)

2025, Radiochimica Acta

TRU resin can be used to rapidly and selectively extract Tc(VII) and Re(VII). The retention capacity curves of Tc(VII) and Re(VII) for HNO3, HCl, H2SO4 and H3PO4 solutions were studied and prepared. Tc(VII) and Re(VII) were simultaneously extracted in 2 M H2SO4 and 1.5 M H3PO4 and were effectively separated from Mo(VI) and Ru(III). Tc(VII) and Re(VII) remained strongly bonded to the resin even after washing using a large volume of 2 M H2SO4 at a relatively high flow rate. Also, they were both completely eluted from the resin using 15 mL of near boiling water, an eluent directly compatible for ICP-MS instrument measurements.

2025, Colloids and Surfaces A: Physicochemical and Engineering Aspects

 1.-A recovery system of chlorpheniramine by Emulsion Liquid Membranes is proposed.  2.-Soy lecithin is a good carrier to perform the transfer of CPM through the ELM.  3.-The system composed of Abil EM90®, soy lecithin and HCl turned out be efficient.  4.-High recovery percentages of CPM and fast transfer rate were obtained.  5.-This application of ELM is a contribution to wastewater treatment.

2025, Journal of Chemical Technology & Biotechnology

BACKGROUNDThis work involved a systematic study of the recovery of ibuprofen (IBP) from aqueous solutions by emulsion liquid membranes (ELM).RESULTSA preliminary liquid–liquid extraction study was performed in order to determine the most appropriate system to extract the IBP. The results show that Parleam 4 and NaOH work very well as extractant and strippant, respectively. The conditions for preparing the ELMs were established. The influence of parameters such as the agitation speed, preparation time and composition of the ELM were evaluated for membrane stability (by laser diffraction) and for IBP recovery efficiency. It was also shown that the influence of trioctylamine (TOA) in the ELM is such that only a low concentration is required to obtain stable and highly efficient membranes.CONCLUSIONThe membrane prepared with Parleam 4 + TOA 0.1% w/V + Abil EM 90 at 5% w/V as organic phase, and NaOH 0.05 mol L‐1, as internal aqueous phase, showed the highest recovery percentages (> 99...

2025, Journal of Chromatography A

An analytical method consisting of extraction, clean-up, and analysis by gas chromatography-electron-capture detection (GC-ECD) was developed for the determination of trichlorobenzenes (TCBs) in fish samples. Two extraction methods, saponification and liquid-liquid extraction (S-LLE), and microwave-assisted extraction (MAE), were evaluated. In both cases, n-pentane was used as the extraction solvent. For S-LLE, the recoveries ranged from 66.669.1% for 1-bromo-4chlorobenzene (4-BCB) to 93.564.9% for 1,2,4-trichlorobenzene (1,2,4-TCB). The recoveries were significantly lower, between 31.063.9% for 1,2,3-trichlorobenzene (1,2,3-TCB) and 52.363.0% for 1,3,5-trichlorobenzene (1,3,5-TCB), in the absence of fish. Proteins and glycerides of the fish tissue seemed to compete with TCBs for the base, and hence decreased their decomposition rate. In the case of MAE, the recoveries were highly dependent on the pressure applied during extraction. At 5 bar, much higher recoveries were obtained, from 66.7615.6% for 4-BCB to 79.9613.6% for 1,2,4-TCB, than at 1 bar. Sulfur formation was, however, observed at 5 bar, and interfered with the GC-ECD analysis of TCBs. Sulfur was adequately removed by copper powder treatment, which was shown not to affect the recovery of analytes. The recoveries of target analytes by S-LLE and MAE did not differ statistically (t-test, a50.01). Both methods were appropriate for the detection of TCBs at concentration levels typically observed in marine biota, i.e. |1 ng / g. S-LLE was, however, more time consuming, and required larger volumes of high-purity organic solvents than MAE.

2025, Chemosphere

Lipophilic organic compounds originating from kraft pulping and papermaking were identified by straight gas chromatography/mass spectrometry (CC/MS) analyses. Samples analyzed included a primary clarifier effluent (PE) and a secondary clarifier effluent (SE) from the activated sludge treatment plant of a Finnish ECF-bleached (Elementally Chlorine Free) kraft pulp and paper mill. Liquid-liquid extraction composition of PE was compared with solid phase extraction (SPE) and dialysis of a semipermeable membrane device (SPMD) exposed to PE. Dichloromethane extracts of particulate material isolated from PE, sludges from both the primary and secondary clarifier, a sediment collected in the vicinity of the mill and whitefish subacutely exposed to the secondary treatment effluent were also investigated. Typical pulp mill-related compounds such as terpenes, terpenoids and aromatic compounds were identified in PE whereas these were non-detectable in SE. For example, thunbergene, thunbergol, squalene, longifolene and derivatives of abietic acid were observed in PE. Alkylated polycyclic aromatics were major compounds identified in the sediment sample with retene (C4alkyl phenanthrene) as a predominant component.

2025, Physical Chemistry Chemical Physics

A membrane based liquid–liquid extraction microfluidic device coupled with X-ray fluorescence enables the first quantification of free energies of transfer dependence for a complex mixture of rare earth elements and iron using synergic... more

2025, Langmuir

We propose the statistical thermodynamic model for the prediction of the liquid-liquid extraction efficiency in the case of rare-earth metal cations using the common bis(2-ethyl-hexyl)phosphoric acid (HDEHP) extractant. In this soft matter-based approach, the solutes are modeled as colloids. The leading terms in free-energy representation account for: the complexation, the formation of a highly curved extractant film, lateral interactions between the different extractant head groups in the film, configurational entropy of ions and water molecules, the dimerization, and the acidity of the HDEHP extractant. We provided a full framework for the multicomponent study of extraction systems. By taking into account these different contributions, we are able to establish the relation between the extraction and general complexation at any pH in the system. This further allowed us to rationalize the well-defined optimum in the extraction engineering design. Calculations show that there are multiple extraction regimes even in the case of lanthanide/acid system only. Each of these regimes is controlled by the formation of different species in the solvent phase, ranging from multiple metal cation-filled aggregates (at the low acid concentrations in the aqueous phase), to the pure acid-filled aggregates (at the high acid concentrations in the aqueous phase). These results are contrary to a long-standing opinion that liquid-liquid extraction can be modeled with only a few species. Therefore, a traditional multiple equilibria approach is abandoned in favor of polydisperse spherical aggregate formations, which are in dynamic equilibrium.

2025, Brazilian Journal of Microbiology

Glucose-6-phosphate dehydrogenase (G6PDH) is an important enzyme used in biochemical and medical studies and in several analytical methods that have industrial and commercial application. This work evaluated the extraction of G6PDH in aqueous two-phase system (ATPS) of poly(ethyleneglycol) (PEG)/phosphate buffer, using as enzyme source a medium prepared through commercial baker's yeast disruption. Firstly, the effects of PEG molar mass on the enzyme partition and of homogenization and rest on the system equilibrium were investigated. Afterwards, several ATPS were prepared using statistical analysis (2 2 factorial design). The results, including kinetic and thermodynamic parameters for the G6PDH activity, showed partial purification of this enzyme in ATPS composed of 17.5% (w/w) PEG400 and 15.0% (w/w) phosphate. A high enzymatic recovery value (97.7%), a high partition coefficient (351), and an acceptable purification factor (2.28 times higher than in cell homogenate) were attained from the top phase. So, it was possible to attain an effective enzyme pre-purification by separating some contaminants with a simple method such as liquid-liquid extraction in aqueous two-phase systems (ATPS).

2025, Energy & Fuels

A method using liquid-liquid extractions has been developed for matrix simplification and evaluated by gel permeation chromatography hyphenated with inductively coupled plasma and mass spectrometry (GPC ICP MS). In this method, maltenes were dissolved in n-heptane (HEP), and extractions with methanol (MeOH), acetonitrile (ACN) and dimethylformamide (DMF) were performed. The extraction with ACN is more efficient than that of MeOH for the removal of compounds with LMW containing V (our reference element) and more selective than that of DMF (with this solvent, compounds with LMW and MMW are extracted). Thus, a sequential extraction was performed by applying ACN to selectively remove LMW compounds, followed by extractions with DMF in the resulting maltene to separate the MMW compounds from the HMW compounds remaining in the final remnant maltene. The results show, for the first time in the literature, that it is possible to separate the three V and Ni species of compounds present in maltenes based on their molecular weight (HMW, MMW and LMW).

2025, Journal of Chromatography B

The determination of the concentrations of antiretroviral drugs in hair is believed to be an important means for the assessment of the long-term adherence to highly active antiretroviral therapy. At present, the combination of tenofovir, lamivudine and nevirapine is widely used in China. However, there was no research reporting simultaneous determination of the three drugs in hair. The present study aimed to develop a sensitive method for simultaneous determination of the three drugs in 2-mg and 10-mg natural hair (Method 1 and Method 2). Hair samples were incubated in methanol at 37 °C for 16 h after being rinsed with methanol twice. The analysis was performed on high performance liquid chromatography tandem mass spectrometry with electronic spray ionization in positive mode and multiple reactions monitoring. Method 1 and Method 2 showed the limits of detection at 160 and 30 pg/mg for tenofovir, at 5 and 6 pg/mg for lamivudine and at 15 and 3 pg/mg for nevirapine. The two methods showed good linearity with the square of correlation coefficient > 0.99 at the ranges of 416-5000 and 77-5000 pg/mg for tenofovir, 12-5000 and 15-5000 pg/mg for lamivudine and 39-50,000 and 6-50,000 pg/mg for nevirapine. They gave intra-day and inter-day coefficient of variation < 15% and the recoveries ranging from 80.6 to 122.3% and from 83.1 to 114.4%. Method 2 showed LOD and LOQ better than Method 1 for tenofovir and nevirapine and matched Method 1 for lamivudine, but there was high consistency between them in the determination of the three drugs in hair. The population analysis with Method 2 revealed that the concentrations in hair were decreased with the distance of hair segment away from the scalp for the three antiretroviral drugs.

2025

Flavonoids: quercitrin, myricitrin and rutin and their metal complexes were comparatively investigated for binding to DNA by means of spectrophotometric methods and DNAse activities were evaluated via agarose gel electrophoresis of pBR322. Free flavonoids bind to DNA in an intercalative mode, but Cu(II) complexes of these flavonoids bind even stronger due to the electrostatic interaction of the metal in addition to the intercalation. Flavonoids show protective effect against DNA cleavage in the presence of peroxide. However, Cu(II) and Zn(II) complexes of these flavonoids cause multiple scissions on the DNA backbone. In addition, Cu(II) complexes of the flavonoids have stronger DNAse activity. Moreover, myricitrin was found two times more cytotoxic when combined with metal ions (Cu2+ or Zn2+) than when used alone against peripheral blood mononuclear cells.

2025

Fibrinolytic proteases produced by Bacillus sp. has attracted interest in the pharmaceutical industry as a promising alternative in thrombolytic therapy due to their effectiveness in degrading fibrin, its production requiring the development of an efficient recovery process. Aqueous two-phase systems (ATPS) have been recognized as an efficient and economical process for recovering enzymes. To optimize the recovery of fibrinolytic protease from the fermentation broth of Bacillus sp. UFPEDA 485, a 2 3 full factorial design was used to evaluate the influence of the three independent variables PEG molar mass (M PEG ), PEG concentration (C PEG ) and sodium sulfate concentration (C Na2SO4 ) on the partition coefficient (K), purification factor (PF) and yield recovery (Y) of fibrinolytic protease in PEG/Na 2 SO 4 aqueous two-phase system. For all ATPS studied, enzymes partitioned to the top phase and the highest extraction was obtained for M PEG 6000 g.mol -1 , C PEG 24 % (w/w) and C Na2SO4 11.6 % (w/w) with K = 5.03; PF = 3.30; Y = 91.40% and Fibrinolytic activity in the top phase 821 U.mL -1 . Findings reported here show that ATPS composed of PEG/Na 2 SO 4 is a valuable strategy for the extraction of fibrinolytic protease and can be considered a promising method for the extraction of enzymes in industrial scale.

2025, Journal of Chromatography A

Staphylococcus aureus is a common pathogen known to cause relatively minor infections as well as severe disorders in humans. Although there is fair amount of published data concerning various aspects of its biology, epidemiology, genetics, etc., there is still a scarce amount of data presenting reliable and thorough investigations regarding high-throughput analysis of total S. aureus lipid content. Therefore, the aim of this study was to develop an analytical method that in combination with advanced chemometric tools enables comprehensive lipidomic analysis of S. aureus cells. The newly developed method uses high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-Q-TOF-MS) to directly examine extracted lipids and further identify them within a newly developed novel S. aureus lipids database. High coverage of the S. aureus lipidome was obtained by simultaneous bacterial cell lysis and liquid-liquid extraction. The combination of three techniques enabled the analysis of the major membrane lipid classes of S. aureus: separation of the lipid extract in reversed-phase mode, Q-TOF-MS detection in positive ion mode, and lipid database mining. The developed lipidomic approach is also a powerful tool that allows one to assess the lipid content of S. aureus cells in a comparative manner between strains characterized by different phenotypic features as exemplified here by their various sensitivities toward antibiotics.

2025, Polycyclic Aromatic Compounds

BACKGROUND: A rapid, selective and sensitive gas chromatographic method is described for the analysis of four fungicides -pyrimethanil, metalaxyl, penconazol and dichlofluanid, widely used in vineyards -in must and wine, as well as samples during alcoholic fermentation. The effect of alcoholic fermentation on pyrimethanil concentration in synthetic and real musts was studied. The proposed method was based on liquid-liquid extraction followed by gas chromatography with nitrogen-phosphorus detector. n-Hexane was the most appropriate solvent for extracting the target fungicides in synthetic and real samples. Quality parameters of the proposed method presented good recovery (ca 78.3% for almost all compounds) and precision (between 1.4% and 6.1%), and quantification limits lower than maximum residue limits. However, for dichlofluanid recovery levels of well over 100% were found. CONCLUSIONS: There was no matrix effect in the analysis of pyrimethanil, metalaxyl or penconazol, but this effect was observed for dichlofluanid in synthetic and real matrices. The application of the fermentative process on pyrimethanil fungicide caused a high decrease in the concentration of this compound, and no product appeared in degradation. The decrease of pyrimethanil in fermented samples was similar in both synthetic and real samples.

2025, Journal of Chromatography B: Biomedical Sciences and Applications

A gas chromatography-mass spectrometry method (SIM mode) was developed for the determination of perfluorodecalin (cis and trans isomers, 50% each) (FDC), and perfluoromethylcyclohexylpiperidine (3 isomers) (FMCP) in rat blood. The chromatographic separation was performed by injection in the split mode using a CP-select 624 CB capillary column. Analysis was performed by electronic impact ionization. The ions m /z 293 and m /z 181 were selected to quantify FDC and FMCP due to their abundance and to their specificity, respectively. The ion m /z 295 was selected to monitor internal standard. Before extraction, blood samples were stored at 2308C for at least 24 h in order to break the emulsion. The sample preparation procedure involved sample clean-up by liquid-liquid extraction. The bis(F-butyl)ethene was used as the internal standard. For each perfluorochemical compound multiple peaks were observed. The observed retention times were 1.78 and 1.87 min for FDC, and 2.28, 2.34, 2.48 and 2.56 min for FMCP. For each compound, two calibration curves were used; assays showed good linearity in the range 0.0195-0.78 and 0.78-7.8 mg / ml for FDC, and 0.00975-0.39 and 0.39-3.9 mg / ml for FMCP. Recoveries were 90 and 82% for the two compounds, respectively with a coefficient of variation ,8%. Precision ranged from 0.07 to 15.6%, and accuracy was between 89.5 and 111.4%. The limits of quantification were 13 and 9 mg / ml for FDC and FMCP, respectively. This method has been used to determine the pharmacokinetic profile of these two perfluorochemical compounds in blood following administration of 1.3 g of FDC and 0.65 g of FMCP per kg body weight, in emulsion form, in rat.

2025, Chemical Engineering and Processing - Process Intensification

 A novel contactor equipped with four 1.7 MHz ultrasound transducers is designed.  Effect of ultrasound and nanoparticles on liquid-liquid mass transfer is considered.  The influence weight fraction of nanoparticles on the mass transfer characteristics is investigated.  Simultaneous use of ultrasound and nanoparticles shows high positive effect on the mass transfer characteristics.  The effect of ultrasound power and the location of ultrasound transducers on the sonoextractor is investigated and optimized conditions are proposed.

2025, Journal of Chromatography B

A simple enantioselective method for the determination of praziquantel (PZQ) and trans-4hydroxypraziquantel (4-OHPZQ) in human plasma was developed and validated by high-performance liquid chromatography/mass spectrometry. The plasma samples were prepared by liquid-liquid extraction using a mixture of methyl-tert-butylether/dichloromethane (2:1, v/v) as extraction solvent. The direct resolution of PZQ and 4-OHPZQ enantiomers was performed on a Chiralpak AD column using hexane-isopropanol (75:25, v/v) as the mobile phase. Diazepam was used as internal standard. The method described here is simple and reproducible. The quantitation limit of 1.25 ng/ml for each PZQ enantiomer and of 12.5 ng/ml for each 4-OHPZQ enantiomer permits the use of the method in studies investigating the kinetic disposition of a single dose of 1.5 g racemic PZQ. Enantioselectivity in the kinetic disposition of PZQ and 4-OHPZQ was observed in the clinical study, with the demonstration of a higher proportion of the (+)-(S)-PZQ and (-)-(R)-4-OHPZQ enantiomers in plasma.

2025, Environmental Monitoring and Assessment

A simple, sensitive and reliable HPLC-FLD method for the routine determination of 4-nonylphenol, 4-NP and 4-tert-octylphenol, 4-t-OP content in water samples was developed. The method consists in a liquid-liquid extraction of the target analytes with dichloromethane at pH 3.0-3.5 followed by the HPLC-FLD analysis of the organic extract using a Zorbax Eclipse XDB C8 column, isocratic elution with a mixed solvent acetonitrile/water 65:35, at a flow rate of 1.0 mL/min and applying a column temperature of 40 • C. The method was validated and then applied with good results for the determination of 4-NP and 4-t-OP in Ialomiţa River water samples collected each month during 2006. The concentration levels of 4-NP and 4-t-OP vary between 0.08-0.17 μg/L with higher values of 0.24-0.37 μg/L in the summer months for 4-NP, and frequently <0.05 μg/L but also between 0.06-0.09 μg/L with higher values of 0.12-0.16 μg/L in July and August for 4-t-OP and were strongly influenced by sesonial and

2025, Journal of Food Science

Chocolate is a key ingredient in many foods such as milk shakes, candies, bars, cookies, and cereals. Chocolate candies are often consumed by mankind of all age groups. The presence of polycyclic aromatic hydrocarbons (PAHs) in chocolate candies may result in health risk to people. A rapid, precise, and economic extraction method was optimized and validated for the simultaneous determination of polycyclic aromatic hydrocarbons in chocolate candy by highperformance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GS-MS) as a confirmatory technique. The method was optimized by using different solvents for liquid-liquid extraction, varying volume of deemulsifying agent, and quantity of silica gel used for purification. The HPLC separation of 16 PAHs was carried out by C-18 column with mobile phase composed of acetonitrile : water (70 : 30) in isocratic mode with runtime of 20 min. Limit of detection, limit of quantification (LOQ), and correlation coefficients were found in the range of 0.3 to 4ng g -1 , 0.9 to 12ng g -1 , and 0.9109 to 0.9952, respectively. The exploration of 25 local chocolate candy samples for the presence of PAHs showed the mean content of benzo[a]pyrene as 1.62 ng g -1 , which representing the need to evaluate effective measures to prevent more severe PAHs contamination in chocolate candies in future.

2025

Results about the kinetics of extraction of Eu(III) and Am(III) by extractants designed for the industrial reprocessing of nuclear wastes are reported. They were obtained using the rotating membrane cell technique (RMC). Extraction and stripping kinetic rate constants were determined for various compositions of the aqueous and organic phases. The transfer was studied at liquid/liquid interfaces between an aqueous nitric acid solution and an organic solvent containing the diglycolamide extractant molecule TODGA, or a mixture of the bipyridine molecule CyMe 4 BTBP with TODGA (the latter being used as a phase-transfer catalyst), dissolved in an aliphatic diluent. In some experiments, an aqueous ligand (a sulfonated bis triazinyl pyridine, SO 3 -Ph-BTP, or a PyTri-diol) was added to the aqueous phase as a stripping agent. The diffusion coefficients of Eu(III) and Am(III), that are key in the analysis of the kinetic data, were measured using the RMC and the closed capillary technique. Whenever possible, mechanisms are proposed to interpret the experimental results.

2025, Journal of Sciences, Islamic Republic of Iran

In the present study, an investigation on the complex formation between mono- and divalent metal ions (Na+, K+, Li+ and Mg2+) in the form of salt with different podands using various solvents has been carried out. Isolated complexes were characterized by different spectroscopic techniques viz. IR, NMR and elemental analysis. On the basis of the obtained data, it was observed that number of donor sites, ionic potential, size fit concept in pseudocyclic cavity etc. are the deciding factors for complexation which make it differ between solid and solution complexation using ionophores.

2025, Journal of Hazardous Materials

• Recycling of rare earth metals from fluorescent lamps was conducted by ionic liquid-mediated extraction. • Acid leaching from a waste phosphor powder was carried out using sulfuric and nitric acids. • An ionic liquid was used as extracting solvent for the rare earth metals. • Selective extraction of rare earth metals from leach solutions was attained. • The extracting ionic liquid phase was recyclable in the recovery process.

2025, Environmental science & technology

Effluents from wastewater treatment systems contain a variety of organic compounds, including end products from the degradation of influent substrates, nonbiodegradable feed compounds, and soluble microbial products (SMPs) produced by microbial metabolism. It is important to identify the major components of these SMPs to understand what is in wastewater effluents. In this study, physical pretreatments to extract and concentrate low molecular weight SMPs (MW< 580 Da) from effluents were optimized. Liquid-liquid extraction (LLE) of a 200 mL effluent sample showed the best performance using a mixture of n-hexane, chloroform, and dichloromethane (70 mL) for extraction. For solid phase extraction (SPE), two OasisHLB cartridges were connected in-line to optimize recovery, and the eluted samples from each cartridge were analyzed separately to avoid overlapping peaks. Four solvents varying from polar to nonpolar (methanol, acetone, dichloromethane, and n-hexane) were selected to maximize...

2025, Industrial & Engineering Chemistry Research

Separation of thorium from zirconium carbide waste is reported. The waste typically contains zirconium, yttrium, uranium, and thorium, along with other impurities including rare earth elements (REEs), iron, calcium, aluminum, hafnium, and titanium. The first step in the separation was selective leaching of zirconium, uranium, and most other impurities with HNO 3 -HF, leaving thorium and REEs as insoluble fluorides. The effective parameters such as HNO 3 and HF concentrations, temperature, and time were optimized for achieving the maximum leaching of zirconium and the minimum leaching of thorium, using central composite design and a multiple response optimization algorithm. Thorium and REEs were leached from the residual solid with H 2 SO 4 , followed by their precipitation with ammonia, dissolution of the precipitate in HNO 3 , and extraction of thorium with tri-noctylamine-kerosene. The factors affecting the extraction of thorium were optimized with respect to HNO 3 , TOA, diluent, V org /V aq , and extraction time. Using the above sample preparation and extraction methods, thorium could be extracted with an efficiency of 95.6%.

2025, International Journal of Biological Macromolecules

Affinity partitioning combines the partitioning behavior of biological macromolecules in aqueous twophase systems with the principle of biorecognition. Among the numerous substances that have been evaluated as ligands, the reactive dyes constitute a group of low cost textile dyes which have proved to act as biomimetic ligands for many enzymes. The ability of reactive yellow 2 (RY2) to interact with trypsin (TRP) and chymotrypsin (ChTRP) and its behavior in aqueous two-phase systems formed by polyethylene glycol (PEG) and sodium citrate (NaCit) -were investigated. Different variables such as PEG molecular weight, tie line length and dye concentration were analyzed. RY2 showed to bind specifically to both TRP and ChTRP with affinity constants near to 10 3 M -1 . Its partition equilibrium is practically displaced to the top phase in systems formed by PEG of different molecular weight. Addition of this dye to PEG 8000/NaCit systems until a final concentration of 0.196% (w/w) induced an increase in TRP and ChTRP partition coefficients of at least 2 times over that in the absence of the ligand. These findings demonstrate that RY2 fulfils all the requirements to be considered as an affinity ligand in aqueous two-phase partitioning of TRP and ChTRP.

2025, Forensic Science International

This paper describes an analytical method for strychnine determination in biological samples by gas chromatography / mass spectrometry and their application in the investigation of two cases involving strychnine ingestion: A fatal case and a clinical one. The strychnine is isolated from biological samples using a liquid-liquid extraction procedure. The clean-up procedure is performed using an acid solution. Papaverine is used as internal standard in the quantification of strychnine. In the analysed specimens, the limits of quantification were 0.1 mg / ml or 0.1 mg/g. The recovery rate ranged from 75.0% to 98.7% and the coefficients of variation ranged from 4.8% to 10.5%.

2025, Analytical Chemistry

Competltlve solvent extractlon of alkall-metal cations from aqueous solutlons Into chloroform by a series of llpophlllc crown ether carboxyllc acids wlth varylng rlng skes is reported. Extractkn selectivity for Ll' Is observed for #pophlHc crown ether carboxyllc a c h whh 12-ltimembered wether rlngs contalnlng four oxygen atoms. For lipophilic 14crown-4-carboxylic acids, very hlgh LI+/Na+ selectlvlty coefflclents of 17-20 are observed wlth no detectable extraction of K+, Rb+, or C s ' . Lipophlllc crown ether carboxylic aclds which contain 15crown-5, 18crown-6, and 21-crown-7 rings exhiblt good selectivltles for Na', K', and Cs', respectlvely. In contrast, poor extractlon selectlvlty is observed for llpophlllc crown ether carboxyllc acids wAh 24-crown-8, 27-crown-9, and 30-crown-10 rings.

2025, Journal of Chromatography B

Qualitative studies are described on the metabolism and the toxicological analysis of the nootropic fipexide (FIP) in rat urine using gas chromatography-mass spectrometry (GC-MS). FIP was extensively metabolized to 1-(3,4-methylenedioxybenzyl)piperazine (MDBP), 4chlorophenoxyacetic acid, 1-[2-(4-chlorophenoxy)acetyl]piperazine, N-(4-hydroxy-3-methoxy-benzyl)piperazine, piperazine, N-(3,4-methylenedioxybenzyl)ethylenediamine, and N-[2-(4-chlorophenoxy)acetyl]ethylenediamine. The authors' systematic toxicological analysis (STA) procedure using full-scan GC-MS after acid hydrolysis of one urine aliquot, liquid-liquid extraction and acetylation allowed the detection of FIP via its metabolites in rat urine after administration of a common FIP dose. Therefore, this qualitative procedure should also be suitable for detection of a FIP intake in human urine. Differentiation of an intake of FIP from that of other drugs which form common metabolites is discussed.

2025, Journal of Chemical and Petroleum Engineering

This study presents a computational fluid dynamics (CFD) simulation of two-phase flow patterns in a Y-shaped microfluidic device. The two-phase flow of water and n-butyl acetate is simulated using the volume of fluid (VOF) method in a Y-shaped microfluidic device with different flow rates. A 2D model was used for simulation, and the results were compared to experimental data, showing good consistency. The study also examined the effects of organic (n-butyl acetate) and flow on the overall flow model. The authors observe three different flow patterns, including slug flow, parallel flow, and droplet flow, depending on the flow rate. The results indicate that a slug flow pattern is detected when the flow rates of the aqueous and organic phases are both low and similar. Nonetheless, as the overall flow rate rises, the slug flow pattern shifts to either parallel droplet or plug flow. Similarly, when the flow rate of the aqueous phase is increased while keeping the organic phase flow rate constant, the shift occurs from slug flow to droplet flow. Therefore, this study is significant in providing insights into the different flow regimes that can occur in a microfluidic system. This understanding can be used to design and optimize microfluidic devices for a variety of applications.

2025, Talanta

Extraction chromatographic (EXC) resins incorporating an appropriate crown ether in an oxygenated organic solvent such as 1-octanol are well established as sorbents for the analytical-scale separation and preconcentration of radiostrontium from a variety of sample types. Recent solvent extraction studies employing crown ethers in various 1-alkyl-3-methylimidazolium-based (CnC1im(+)) room-temperature ionic liquids (RTILs) indicate that under certain conditions, distribution ratios (DSr) for strontium far in excess of those observed with conventional organic solvents are observed. To determine if this increase in liquid-liquid extraction efficiency will lead to improved strontium sorbents, several EXC resins and sol-gel glasses incorporating di-tert-butylcyclohexano-18-crown-6 (DtBuCH18C6) in either 1-decyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (C10C1imTf2N) or the related hydroxyalkyl-functionalized IL 1-(12-hydroxydodecyl)-3-butylimidazolium bis[(trifluoromethyl)su...

2025, Separation Science and Technology

2025, Journal of the Brazilian Chemical Society

2025, Science of The Total Environment

Chemicals showing structural or functional similarity to bisphenol A (BPA), commonly called BPA analogues, have recently drawn scientific attention due to their common industrial and commercial application as a substitute for BPA. In the European Union, the use of BPA has been severely restricted by law due to its endocrine disrupting properties. Unfortunately, it seems that all BPA analogues show comparable biological activity, including hormonal disruption, toxicity and genotoxicity. Until now, the knowledge about human exposure to BPA analogues is scarce, mainly due to the lack of the data concerning their occurrence in human derived biological samples. This study presents the development of an analytical method for determination of trace levels of eleven BPA analogues in human blood serum samples. The method involves fast and simple liquid-liquid extraction, using low sample and solvent volumes. Chromatographic separation of analytes was optimized using onefactor-at-a-time approach (mobile phase composition, gradient shape, chromatographic column selection, separation temperature, etc.). The method allows for effective separation of the analytes, even in the case of configurational isomers (bisphenol M and bisphenol P). The calibration curves for all analytes were linear in the range tested. The limits of detection and quantitation were in the range of 0.0079 ÷ 0.039 ng/mL and 0.024 ÷ 0.12 ng/mL respectively. Compounddependent recovery values were in the rage of 88 ÷ 138%. Matrix effects were mitigated with the help of matrix-matched calibration curves prepared for every batch of samples. Results obtained after the analysis of 245 real human blood serum samples indicate that human beings are exposed to different BPA analogues, that are present in the environment and in common, daily use products.

2025, The Science of the total environment

2025, Trends in Analytical Chemistry

-Trends in automation of liquid-liquid extraction (LLE) in radiochemical analysis -Trends in automation of Solid Phase Extraction (SPE) in radiochemical analysis -Pros and cons of automation of radiochemical analysis by flow analysis... more

2025, Environmental science and pollution research international

This study presents computational fluid dynamics (CFD) simulation of dispersion-free liquid-liquid extraction of copper(II) with trifluoroacetylacetone (TFA) in hollow fiber membrane contactor (HFMC). Mass and momentum balance Navier-Stokes equations were coupled to address the transport of copper(II) solute across membrane contactor. Model equations were simulated using COMSOL Multiphysics™. The simulation was run to study the detailed concentration distribution of copper(II) and to investigate the effects of various parameters like membrane characteristics, partition coefficient, and flow configuration on extraction efficiency. Once-through extraction was found to be increased from 10 to 100% when partition coefficient was raised from 1 to 10. Similarly, the extraction efficiency was almost doubled when porosity to tortuosity ratio of membrane was increased from 0.05 to 0.81. Furthermore, the study revealed that CFD can be used as an effective optimization tool for the development...

2025, Journal of Pharmaceutical and Biomedical Analysis

 First LC-MS/MS method being reported for the simultaneous quantification of darolutamide and ORM-15341 in mice plasma.  Simple sample processing method and shorter run time (2.5 min) enables this method as a high throughput assay.  Method was validated as per regulatory guidelines.  The method is specific, precise, accurate and no matrix effect was observed and linear from 0.61-1097 ng/mL for both the analytes.  Method was used in a mice pharmacokinetic study to derive the pharmacokinetic parameters for darolutamide and ORM-15341.

2025, Bioresource Technology

The production of acetone, butanol, and ethanol (ABE) by fermentation is a process that had been used by industries for decades. Two stage immobilized column reactor system integrated with liquid-liquid extraction was used with immobilized Clostridium acetobutylicum DSM 792, to enhance the ABE productivity and yield. The sugar mixture (glucose, mannose, galactose, arabinose, and xylose) representative to the lignocellulose hydrolysates was used as a substrate for continuous ABE production. Maximum total ABE solvent concentration of 20.30 g.L -1 was achieved at a dilution rate (D) of 0.2 h -1 , with the sugar mixture as a substrate. The maximum solvent productivity (10.85 g.L -1 h -1 ) and the solvent yield (0.38 g.g -1 ) were obtained at a dilution rate of 1.0 h -1 . The maximum sugar mixture utilization rate was achieved with the present set up which is difficult to reach in a single stage chemostat. The system was operated for 48 days without any technical problems.

2025, Talanta

Esterase activity found in muscle extracts is useful to evaluate harmful effects of anticholinesterase pollutants. Yet, most procedures applied in the extraction of fish muscle esterases in order to investigate their activity as a biomarker of environmental exposure comprise the homogenization of muscle tissue in low-salt solutions, followed by centrifugation to separate the supernatant as the enzyme source. However, acetylcholinesterase (AChE), the main target in these monitoring efforts, is a membrane-bound protein and is only present in muscle extracts if homogenization is carried out using chaotropic high-salt solutions. In this context, four extraction procedures using muscle tissue from six fish species were evaluated in order to establish a reproducible and reliable AChE assay for the determination of this biomarker. Results indicate that over 80% of AChE activity might be lacking in low-salt supernatants, and that the highest activities are obtained after extraction with sol...

2025, Biomedical Chromatography

In vivo absorption and oxidative metabolism of salicylic acid in rat small intestine was studied by luminal perfusion experiment. Perfusion through the lumen of proximal jejunum with isotonic medium containing 250 µM sodium salicylate was carried out. Absorption of salicylate was measured by a validated HPLC-DAD method which was evaluated for a number of validation characteristics (specificity, repeatability and intermediate precision, limit of detection, limit of quantification, linearity and accuracy). The method was linear over the concentration range 0.5-50 µg/mL. After liquid-liquid extraction of the perfusion samples oxidative biotransformation of salicylate was also investigated by HPLC-MS. The method was linear over the concentration range 0.25-5.0 µg/mL. Two hydroxylated metabolites of salicylic acid (2,5-dihydroxybenzoic acid and 2,3-dihydroxybenzoic acid) were detected and identified. The mean recovery of extraction was 72.4% for 2,3-DHB, 72.5% for 2,5-DHB and 50.1% for salicylic acid, respectively. The methods were successfully applied to investigate jejunal absorption and oxidative metabolism of sodium salicylate in experimental animals. The methods provide analytical background for further metabolic studies of salycilates under modified physiological conditions.

2025, Journal of Polymers and The Environment

Two new copolymers containing pendant calix[4]arene units with nitrile functionalities at their lower rim have been synthesized via nucleophilic substitution reactions involving... more

Two new copolymers containing pendant calix[4]arene units with nitrile functionalities at their lower rim have been synthesized via nucleophilic substitution reactions involving 5,11,17,23-tetra-tert-butyl-25,27-bis(cyanomethoxy)-26,28-dihydroxy-calix[4]arene (3) or 25,27-bis(cyanometh oxy)-26,28-dihydroxy-calix[4]arene (4) with 1,5-dibromopentane and bisphenol-A. The phase transfer studies were performed by using liquid–liquid extraction procedures. It has been deduced from the observations that both copolymers show a good phase transfer affinity toward

2025, Analytical Sciences

Liquid-liquid extraction of lanthanide ions (Ln 3+ ) using N,N-dioctyldiglycolamic acid (DODGAA) was comprehensively investigated, together with fluorescence spectroscopic characterization of the resulting extracted complexes in the organic phase. DODGAA enables the quantitative partitioning of all Ln 3+ ions from moderately acidic solutions, while showing selectivity for heavier lanthanides, and provides remarkably high extraction separation performance for Ln 3+ compared with typical carboxylic acid extractants. Furthermore, the mutual separation abilities of DODGAA for light lanthanides are higher than those of organophosphorus extractants. Slope analysis, loading tests, and electrospray ionization mass spectrometry measurements demonstrated that the transfer of Ln 3+ with DODGAA proceeded through a proton-exchange reaction, forming a 1:3 complex, Ln(DODGAA)3. The stripping of Ln 3+ from the extracting phase was successfully achieved under acidic conditions. Time-resolved laser-induced fluorescence spectroscopy revealed that the extracted Eu 3+ ions were completely dehydrated by complexation with DODGAA.

2025, Molecules

"Food waste remains a critical global concern, with approximately one third of all food produced being ultimately discarded. Therefore, it is urgent to develop new techniques for the effective repurpose of waste. Aqueous two-phase systems (ATPSs) stand out as a simple and biocompatible liquid-liquid extraction technique for the recovery of bioactive substances from food waste. In ATPSs, the target species partition between two liquid phases, according to affinity, which facilitates its extraction. This work aimed at extracting three polyphenols-chlorogenic acid (CA), ferulic acid (FA), and resveratrol (RV)-through the application of eco-friendly ATPSs composed of water, ethyl lactate (EL), and organic salts, namely disodium succinate (Na 2 Succinate) and disodium tartrate (Na 2 Tartrate), for future application in the valorisation of food waste. All partitions presented successful results, with values of partition coefficients (K) higher than 1 and extraction efficiencies (E) higher than 50%, indicating a preferential migration of the polyphenols to the top phase. The extraction of FA using the ATPS based on Na 2 Tartrate presented the most promising results, with K = 19 ± 6 and E = (94.2 ± 0.9)% for the longest tie-line. Additionally, a comparison with previous works of the research group was drawn, with the extraction of RV exhibiting outstanding performance across all studied ATPSs. Therefore, the assessed ATPSs were shown to hold immense potential for the recovery of polyphenols."

2025, MATEC web of conferences

In this work, the experimental liquid-liquid equilibrium (LLE) data were measured for quaternary mixtures of eugenol(1) + β-caryophyllene(2) + 1-propanol(3) + water(4) at temperatures 303.15, 313.15, and 323.15 K and at atmospheric pressure. The equilibrium data ware determined by using an equilibrium cell with temperature controlled. Quantitive analysis was performed by using gas chromatography (GC) equipped with thermal conductivity detector and capillary column Rtx-5. The experimental data were then correlated by using the NRTL and the UNIQUAC models. The reliability of these models were tested by compared with the experimental results using a root mean square deviation (RMSD). Based on the RMSD, the NRTL and the UNIQUAC models suited really well and give satisfactory result for the system of eugenol, β-caryophyllene, 1-propanol, and water with the average RMSD of the UNIQUAC and the NRTL models were 0.417% and 0.502%, respectively. Furthermore there was no significant effect of temperatures on the equilibrium composition for the system.

2025, Fermentation

Anhydrous ethanol is a promising alternative to gasoline in fuel engines. However, since ethanol forms an azeotrope with water, high-energy-consumption separation techniques such as azeotropic distillation, extractive distillation, and molecular sieves are needed to produce anhydrous ethanol. This work discusses the potential development of an integrated process for bioethanol production using ionic liquids and Ceratonia siliqua as a carbohydrate source for further fermentation of the aqueous extracts. A four-stage counter-current system was designed to improve the sugar extraction yield to values close to 99%. The alcoholic fermentation of the extracts showed ethanol concentrations of 95 g/L using the microorganism Saccharomyces cerevisae. The production of anhydrous ethanol through extractive distillation with ethylene glycol was simulated using CHEMCAD software, with an energy consumption of 13.23 MJ/Kg of anhydrous ethanol. Finally, several ionic liquids were analyzed and are pr...

2025, Revista de Metalurgia

This work focuses on general guidelines to be considered for application of least-squares routines and artificial neural networks (ANN) in the estimation of metal distribution equilibria in liquid-liquid extraction process. The goal of the procedure in the statistical method is to find the values of the equilibrium constants (K¡) for the reactions involved in the metal extraction which minimizes the differences between experimental distribution coefficient (Dgxp) and theoretical distribution coefficients according to the mechanism proposed (Dt^^gor)-Iri the first part of the article, results obtained with the most frequently routine reported in the bibliography are compared with those obtained using the algorithms previously discussed. In the second part, the main features of a single back-propagation neural network for the same purpose are discussed, and the results obtained are compared with those obtained with the classical methods.

2025, Phytochemistry

The main odorant constituents of Cedrus atlantica essential oil were characterized by GC-Olfactometry (GC-O), using the Aroma Extract Dilution Analysis (AEDA) methodology with 12 panelists. The two most potent odor-active constituents were vestitenone and 4-acetyl-1-methylcyclohexene. The identification of the odorants was realized by a detailed fractionation of the essential oil by liquid-liquid basic extraction, distillation and column chromatography, followed by the GC-MS and GC-O analyses of some fractions, and the synthesis of some non-commercial reference constituents.

2025

Processes of post combustion CO2 capture using amine based solvents generate nitrogenous compounds. Among these products, carcinogenic nitrosamines are of great concern due the potential impacts on the environment and human health. Trace analysis of nitrosamines in simple matrices such as water is well described in standard methods[1] However, measuring nitrosamines in CO2 capture processes matrices is much more challenging since nitrosamines, which are formed to small concentrations as solvent degradation products, may be present in solvent, wash waters, and atmospheric emissions. Within the FP7 OCTAVIUS project, 2 international round robins on the analysis of 9 nitrosamines in solvent matrices and the atmospheric emissions from the EnBW pilot plant in Heilbronn (Germany) were organized. The first round robin test was performed on solvent matrices. The analytical methods of the laboratories involved were compared using synthetic spiked samples and real liquid samples obtained from ...