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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]

7α-Hydroxy-4-cholesten-3-one (C4) is the common intermediary of both primary bile acids. C4 is recommended by the British Society of Gastroenterology for the investigation of bile acid diarrhoea (BAD) in patients with chronic diarrhoea. This project aimed to develop and validate an assay to quantitate C4 in serum and assess the stability of C4 in unseparated blood.Accuracy was underpinned by calibrating to quantitative nuclear magnetic resonance analysis. C4 was analysed in a 96-well plate format with a deuterated C4 internal standard and liquid-liquid extraction. Validation followed the 2018 Food and Drug Administration guidelines. To assess C4 stability, healthy volunteers (n=12) donated 8 fasted samples each. Samples were incubated at 20 °C for up to 72 h and retrieved, centrifuged, aliquoted and frozen for storage at different time points prior to C4 analysis.The C4 method demonstrated excellent analytical performance and passed all validation criteria. The method was found to be accurate, precise, free from matrix effects and interference. After 72 h of delayed sample separation, C4 concentration gradually declined by up to 14 % from baseline. However, the change was not significant for up to 12 h.We present a robust method of analysing serum C4, offering a convenient alternative to 75SeHCAT for BAD investigation. C4 was found to decline in unseparated blood over time; however, after 12 h the mean change was <5 % from baseline. Our results suggest C4 is suitable for collection from both primary and secondary care prior to gastroenterology referral. [ABSTRACT FROM AUTHOR]

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

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

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

The present work is focus on development of anti-psoriasis activity of Karanjin (isolated from Pongamia pinnata seed oil) loaded liposome based lotion for enhancement of skin permeation and retention. Karanjin was isolated using liquid-liquid extraction method and characterised by HPLC analysis and partition coefficient. Further, isolated Karanjin was loaded into liposomes using thin-film hydration technique and optimised by Box-Behnken design. Selected optimised batch was characterised their mean diameter, PDI, zeta potential, and entrapment efficiency, morphology (by TEM), FTIR and ex-vivo skin retention. Additionally, Karanjin loaded liposomes were formulated into lotion and characterise their rheological, spreadability, texture, ex-vivo skin permeation & retention, stability and anti-psoriatic activity in mouse tail model. The yield of Karanjin from seed oil was 0.1% w/v and have lipophilic nature. The optimised liposomal formulation showed 195 ± 1.8 nm mean diameter, 0.271 ± 0.02 PDI, −27.0 ± 2.1 mV zeta potential and 61.97 ± 2.5% EE. TEM image revel the spherical shap of liposome surrounded by single phospholipid bilayer and no interection between drug and excipients. Further, lotion was prepared by 0.1% w/v carbopol and found to 615 mPa.sec viscosity, good thixotropic behaviour, spreadability and texture. There was 22.44% increase in drug permeation for Karanjin loaded liposomal lotion compared to pure Karanjin lotion, confirm by ex-vivo permeation and retention. While, in-vivo study revel the liposomal lotion of Karanjin was found to have 16.09% higher drug activity then 5% w/w conventional Karanjin lotion. Karanjin loaded liposomal lotion have an effective anti-psoriatic agent and showed better skin permeation and retention than the conventional Karanjin lotion. [ABSTRACT FROM AUTHOR]

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

Combined extraction of nickel and cobalt from nickel chloride solution using di (2-ethylhexyl) phosphonic acid(P204) and triisooctylamine(N235) as extractants was studied. The effects of organic phase P204 volume fraction, phase ratio, solution pH, saponification rate, organic phase N235 volume fraction, Cl- mass concentration, and reaction temperature on the purification and impurity removal of nickel chloride solution were investigated. The results show that after removing impurities by P204 extraction, N235 is used to extract cobalt and molybdenum from P204 raffinate, the mass concentrations of Ni2+ is 218.10 g/L, and the mass concentrations of Cu2+, Fe3+, Co2+, and Zn2+ in the residual solution 1.1, 1.2, 1.0 and 0.1 mg/L, respectively, under the conditions of 20% volume fraction of P204 in the organic phase of the P204 extraction and impurity removal process, VO/VA = 1.5/1, raw material solution pH = 3.5, saponification rate of 50%, reaction temperature of 40--50 °C, and N235 volume fraction of 16% in the organic phase of the N235 extraction process, VO/VA=1.2/1, Cl- mass concentration ≥280 g/L, reaction temperature of 40~50 °C, P204 Raffinate pH=3.0, and hydrochloric acid acidification concentration of 3 mol/L, which can meet the requirements of producing high quality electrodeposited nickel cathodes. [ABSTRACT FROM AUTHOR]

BACKGROUND: The leaves of guabirobeira contain important phenolic and flavonoid compounds, known for their antioxidant, anti‐inflammatory, antibacterial, and antinociceptive activities. The purpose of this work was to obtain extracts from guabirobeira leaves through aqueous infusion and pressurized liquid extraction with water, ethanol, and a combination of water–ethanol (ratio 1:1, v/v; PLE‐W:E). Subsequently, we used liquid chromatography coupled with mass spectrometry to identify the chemical compounds, and to study the antioxidant activity in rat brain cells; thiobarbituric acid reactive substances (TBARS) and reactive oxygen species (ROS) antibacterial activity against Gram‐negative and Gram‐positive bacteria were also seen. RESULTS: According to the findings, all four extracts contained a significant amount of phytochemical compounds. Among them, the PLE‐W:E extract showed a higher concentration of flavonoids, demonstrating significant antioxidant activity in in vitro assays of TBARS and ROS in rat brain cells. It also exhibited antibacterial activity against both Gram‐positive and Gram‐negative bacteria. CONCLUSION: Guabirobeira leaf extracts hold promise as a potential source of bioactive compounds. These extracts can be applied across various sectors, including cosmetics and skincare products, pharmaceuticals, food and beverages, natural preservatives, and functional materials. By exploring these potential applications, valuable contributions can be made to the field of sustainable chemistry and pharmacy, furthering the utilization of guabirobeira leaf extracts in diverse industries. This approach also aligns with the promotion of environmentally friendly and sustainable practices. © 2024 Society of Chemical Industry (SCI). [ABSTRACT FROM AUTHOR]

In the present investigation, a total of 108 combinations of ionic liquids (ILs) were screened using the conductor-like screening model for real solvents (COSMO-RS) with the aid of six cations and eighteen anions for the extraction of succinic acid (SA) from aqueous streams through dispersive liquid–liquid microextraction (DLLME). Using the screened ILs, an ionic liquid-based DLLME (IL-DLLME) was developed to extract SA and the role of different reaction parameters in the effectiveness of IL-DLLME approach was investigated. COSMO-RS results suggested that, quaternary ammonium and choline cations form effective IL combinations with [OH¯], [F¯], and [SO42¯] anions due to hydrogen bonding. In view of these results, one of the screened ILs, tetramethylammonium hydroxide [TMAm][OH] was chosen as the extractant in IL-DLLME process and acetonitrile was adopted as the dispersive solvent. The highest SA removal efficiency of 97.8% was achieved using 25 μL of IL [TMAm][OH] as a carrier and 500 μL of acetonitrile as dispersive solvent. The highest amount of SA was extracted with a stir time of 20 min at 300 rpm, followed by centrifugation for 5 min at 4500 rpm. Overall, the findings showed that IL-DLLME is efficient in extracting succinic acid from aqueous environments while adhering to the first-order kinetics. [ABSTRACT FROM AUTHOR]

Rationale: Himalayan marmot oil (SPO) has been used for pharmaceutical purposes for centuries, but its composition is still unclear. The bioactivity of SPO highly depends on the techniques used for its processing. This study focused on the comprehensive lipidomics of SPO, especially on the ones derived from dry rendering, wet rendering, cold pressing, and ultrasound‐assisted solvent extraction. Methods: We performed lipid profiling of SPO acquired by different extraction methods using ultrahigh‐performance liquid chromatography Q‐Exactive Orbitrap mass spectrometry, and 17 classes of lipids (2 BMPs, 12 LysoPCs, 9 LysoPEs, 41 PCs, 24 PEs, 23 Plasmenyl‐PCs, 10 Plasmenyl‐PEs, 10 MGs, 63 DGs, 187 TGs, 2 MGDGs, 3 Cer[NDS]s, 22 Cer[NS]s, 2 GlcCer[NS]s, 14 SMs, 14 CEs, and 6 AcylCarnitines) were characterized. Results: Fifty‐five lipids were differentially altered (VIP > 1.5, p < 0.05) between the extraction techniques, which can be used as potential biomarkers to differentiate SPO extracted by various methods. Additionally, the contents of oleic acid and arachidic acid were abundant in all samples that may suggest their medicinal values and are conducive to in‐depth research. Conclusions: These findings reveal the alterations of lipid profile and free fatty acid composition in SPO obtained with different extraction methods, providing a theoretical foundation for investigating its important components as functional factors in medicines and cosmetics. [ABSTRACT FROM AUTHOR]

AbstractMicroalgal, species are recognized for their high protein content, positioning them as a promising source of this macronutrient. Spirulina platensis, in particular, is noteworthy for its rich protein levels (70 g/100 g dw), which are higher than those of meat and legumes. Incorporating this microalgae into food can provide various benefits to human health due to its diverse chemical composition, encompassing high amount of protein and elevated levels of minerals, phenolics, essential fatty acids, and pigments. Conventional techniques employed for protein extraction from S. platensis have several drawbacks, prompting the exploration of innovative extraction techniques (IETs) to overcome these limitations. Recent advancements in extraction methods include ultrasound-assisted extraction, microwave-assisted extraction, high-pressure-assisted extraction, supercritical fluid extraction, pulse-electric field assisted extraction, ionic liquids assisted extraction, and pressurized liquid extraction. These IETs have demonstrated efficiency in enhancing protein yield of high quality while maximizing biomass utilization. This comprehensive review delves into the mechanisms, applications, and drawbacks associated with implementing IETs in protein extraction from S. platensis. Notably, these innovative methods offer advantages such as increased extractability, minimized protein denaturation, reduced solvent consumption, and lower energy consumption. However, safety considerations and the synergistic effects of combined extraction methods warrant further exploration and investigation of their underlying mechanisms. [ABSTRACT FROM AUTHOR]

Papain a protease enzyme naturally present in the Carica papaya has gained significant interest across several industries due to its unique properties and versatility. The unique structure of papain imparts the functionality that assists in elucidating how papain enzyme works and making it beneficial for a variety of purposes. This review highlights recent advancements in papain extraction techniques to enhance production efficiency to meet market demand. The extraction of papain from the Carica papaya plant offers various advantages such as cost‐effectiveness, biodegradability, safety, and the ability to withstand a wide range of pH and temperature conditions. Key findings reveal that non‐conventional papain extraction techniques offer significant advantages in terms of efficiency, product quality, and environmental sustainability. Furthermore, papain treatment enhances the value of final products due to its anti‐bacterial, anti‐oxidant, and anti‐obesity properties. The ability of papain to hydrolyze a wide range of proteins across various conditions makes it a suitable protease enzyme. While the study emphasizes the advantages of papain, the study also acknowledges limitations such as the continuous research and development to optimize extraction processes which will help unlock papain's potential and meet the growing demand. © 2024 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

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

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

Furosemide (FUR), banned in sports events by the World Anti‐Doping Agency, is a key target in drug tests, necessitating a pretreatment material capable of selectively, rapidly, and sufficiently separating/enriching analytes from complex matrices. Herein, a metal‐mediated magnetic molecularly imprinted polymer (mMIP) was rationally designed and synthesized for the specific capture of FUR. The preparations involved the utilization of chromium (III) as the binding pivot, (3‐aminopropyl)triethoxysilane as functional monomer, and Fe3O4 as core, all assembled via free radical polymerization. Both the morphologies and adsorptive properties of the mMIP were characterized using multiple methods. The resulting Cr(III)‐mediated mMIP (ChM‐mMIP) presented excellent selectivity and specificity toward FUR. Under optimized conditions, the adsorption capacity reached 128.50 mg/g within 10 min, and the imprinting factor was 10.41. Moreover, it was also successfully applied as a dispersive solid‐phase extraction material, enabling the detection of FUR concentration as low as 20 ng/mL in human urine samples when coupled with a high‐performance liquid chromatography/photodiode array. Overall, this study offers a valuable strategy for the development of novel recognition material. [ABSTRACT FROM AUTHOR]

Biobased volatile fatty acid (VFA) production from anaerobic digestion (AD) using extractive fermentation is a promising approach to control the inhibitory effects of acid accumulation in active digesters while producing a second valuable product stream. Five extractants (tri-n-octylamine, tri-n-butyl phosphate, tri-n-octylphosphine oxide, Aliquat 336 and trihexyl(tetradecyl)phosphonium bis-2,4,4-(trimethylpentyl)phosphinate) in combination with oleyl alcohol, lamp oil or canola oil as diluents were investigated based on (i) extraction capacity, (ii) biocompatibility and (iii) feasibility of VFA back extraction. Liquid–liquid extraction with VFA solutions revealed solvents with the capacity to extract acids within pH ranges suitable for AD. Bench-scale biogas experiments demonstrated that biocompatible extractant-solvent systems allow the co-production of biogas and VFAs while enhancing biogas productivity. Solvents were back-extracted using NaOH(aq) to recover VFAs and regenerate the solvent. The novel methodology implemented here could be considered in the development of pH control strategies for the partial removal of VFAs from AD systems while improving the stability of methane production, promoting resource recovery, integrated waste management, waste reduction and utilisation of renewable energy. [ABSTRACT FROM AUTHOR]

The first example of a heteroditopic receptor capable of cooperative recognition and extraction of ammonium salt (NH4X) ion-pairs is described. Consisting of a bidentate 3,5-bis-tellurotriazole chalcogen bond donor binding cleft, the appendage of benzo-15-crown-5 (B15C5) substituents to the tellurium centres facilitates binding of the ammonium cation via a co-facial bis-B15C5 sandwich complex, which serves to switch on chalcogen bonding-mediated anion binding potency. Extensive quantitative ion-pair recognition 1H NMR titration studies in CD3CN/CDCl3 (1 : 1, v/v) solvent media reveal impressive ion-pair binding affinities towards a variety of ammonium halide, nitrate and thiocyanate salts, with the heteroditopic receptor displaying notable ammonium halide salt selectivity. The prodigious solution phase NH4X recognition also translates to efficient solid–liquid and liquid–liquid extraction capabilities. [ABSTRACT FROM AUTHOR]

AbstractNucleosides and nucleobases in edible mushrooms collected from the Tekirdağ region of Turkey were determined by high performance liquid chromatography (HPLC). Separation of compounds was accomplished by gradient elution on a C18 column. A mixture of methanol (MeOH):50 mM sodium phosphate buffer (1:99, v/v) at pH 3.70 and methanol:50 mM sodium phosphate buffer (20:80) at pH 6.20 was used as the solvent. Two methods were used to treat the lyophilized mushrooms: ultrasound-assisted solid-liquid extraction (US-SLE) and pressurized (accelerated) solid-liquid extraction (PSLE). Deionized water was used as the extraction solvent. The extraction temperature and time were optimized. Fourteen nucleosides and nucleobases were simultaneously monitored at 254 nm within 25 min. Ultrasound-assisted solid-liquid was demonstrated to be more effective, perhaps because the pressurized liquid extraction system is a closed system and the matrix-solvent interaction may be insufficient. Adenosine, guanosine and uridine were the most abundant compounds in all studied mushrooms. [ABSTRACT FROM AUTHOR]

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

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

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

This study presents a method based on acid transesterification and the purification by solid-phase extraction (SPE) coupled with gas chromatography–tandem mass spectrometry for quantifying 3- and 2-monochloropropanediol esters (3-MCPDE, 2-MCPDE) and glycidyl esters (GE) in nutritional foods. The fat was extracted by liquid–liquid extraction with petroleum ether and diethyl ether after the sample was hydrolysed with ammonia. Then the extract was purified by a SPE cartridge filled with the aminopropyl sorbents. It was demonstrated that the optimal elution volume for 3-MCPDE, 2-MCPDE and GE greatly depended on the sample matrix and varied from 6 to 12 mL for four different kinds of food matrices. All three analytes in the sample solution could be fully collected in the first 10–12 mL of eluate. By this way, monoacylglycerols commonly present in the samples were fully removed. Therefore, the overestimation of GE quantification was effectively eliminated. The modified analytical procedure was fully validated in a single laboratory and has been recommended as a Chinese Food Safety National Standard. In addition, two derivatisation agents, heptafluorobutyrylimidazole and phenylboronic acid, were proved to be equivalent in method accuracy and precision for the quantification of three analytes. [ABSTRACT FROM AUTHOR]

2-Phenoxyethanol (PhE) is widely used as a preservative in consumer products such as cosmetics as well as at the workplace as a component of metal-working fluids and hydraulic fluids. Therefore, both industry workers and consumers may potentially be exposed to PhE. An analytical method for the quantification of PhE and three selected metabolites, namely phenoxyacetic acid (PhAA), 4-hydroxyphenoxyacetic acid (4-OH-PhAA), and 4-hydroxyphenoxyethanol (4-OH-PhE), in human urine and blood was developed and validated. The sample preparation includes enzymatic hydrolysis of urine samples or protein precipitation of blood samples, followed by liquid – liquid extraction and silylation of the target analytes. Analyses of the extracts were carried out by gas chromatography with tandem mass spectrometry (GC – MS-MS). 3,4-Hydroxyphenoxyethanol, a probably minor PhE metabolite, could not be reliably analyzed due to its instability. The limits of quantification (LOQ) of the analytes ranged between 0.5 and 6.1 μg/L and 2.0 and 3.9 μg/L in urine and blood, respectively. The method was successfully applied to spot urine samples of 50 individuals without occupational exposure to PhE and additionally to blood samples from seven volunteers. In urine, PhAA and 4-OH-PhAA could be quantified in all analyzed samples, whereas 4-OH-PhE and unchanged PhE were found in 36% and 32% of the samples, respectively. In blood, PhAA was also found in every sample in levels above the LOQ, whereas PhE itself was detected in three of seven samples only. Neither 4-OH-PhAA nor 4-OH-PhE was found in any of the analyzed blood samples. The developed method promises to be a valuable tool for PhE monitoring of urine and blood samples and may also enable an advanced investigation of PhE biotransformation pathways in humans. [ABSTRACT FROM AUTHOR]

In this study, a new method was developed for extraction and determination of polycyclic aromatic hydrocarbons (PAHs) in biota samples. The biota samples were packed inside a porous membrane bag and subjected to ultrasonication-assisted solvent extraction. This method showed good applicability to both low and high sample weights. The effect of various parameters such as type and volume of extraction solvent, ultrasonication time, sample weight, and dimensions of extraction device on extraction performance was evaluated. The developed method showed a good linear range from 12.5 to 100 ng/g for all the selected analytes with correlation coefficients ranging from 0.9907 to 0.9999. The limits of detection ranged from 0.97 to 3.47 ng/g. The method's precision was assessed based on relative standard deviations, which were below 13.5% indicating an acceptable precision. The developed procedure used for determination of PAHs in biota samples is characterized by many positive features. The packing of dried biota samples inside the membrane bag is advantageous because it eliminates several steps such as filtration or centrifugation and further extract purification. As the samples are protected inside the membrane bag, they can be easily separated from the solvent extract after the completion of the extraction process by simply removing the membrane bag. Moreover, the membrane may hinder the transportation of macromolecules to the extract, thus resulting in a relatively cleaner extract. Due to its simplicity and excellent figures of merit, this method presents a better potential for routine analysis of polycyclic aromatic hydrocarbons in biota samples. [ABSTRACT FROM AUTHOR]

90Sr is one of the most monitored fission products. New efficient methods for strontium separation are therefore sought. Over the past 20 years, crown ethers solutions in ionic liquids (ILs) have been confirmed to efficiently extract strontium from acidic solutions. Despite all the work done in this field, the extraction mechanism is still not completely clear. Depending on experimental conditions, the extraction is believed to proceed either in the form of an ion-association complex [Sr·CE·(NO3)2] or via exchange between [Sr·CE]2+ and two IL cations. This work aims to study the influence of several extraction parameters and compare them with the presumed mechanisms. [ABSTRACT FROM AUTHOR]

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

Aim: A precise, linear and specific liquid chromatography-tandem mass spectrometry procedure was executed and subjected for validation for the quantification of plasma. Materials and Methods: The chromatography elution was carried out using a C18-Discovery column of 15 cm in length and 2.1 mm in internal diameter, packed with stationary phase particles of 5 µm size, at a flow rate of 0.80 mL/min. An isocratic elution process was conducted with a mobile phase solution consisting of methanol and 0.10% V/V HCOOH in a ratio of 90:10. The separation of Abametapir and Metformin was achieved by a liquid-liquid extraction process using ethyl acetate as the solvent. Results: A triple quadrupole mass spectrometer was used for the measurement of ions. Electrospray ionization is a technology that ionizes positively, and it was used in Multiple Reaction Monitoring (MRM) with parent/product ionic transitions m/z 185.1→106.06 for Abametapir and 130.1→60.20 for the Metformin internal standard. A calibration graph was constructed with values ranging from 2.05 to 82.00 ng/mL, resulting in the equation y=0.0149x+0.00221, with a r2 value above 0.99. The recovery values of Abametapir exceeded 94.27%, with its accuracy assessed in terms of relative error ranging from -4.04% to 6.52%. Conclusion: The accuracy, recovery and sensitivity values of Abametapir in the plasma sample, as shown by the established approach, highlight its significance in pharmacokinetic and bioequivalence research. [ABSTRACT FROM AUTHOR]

The results of scientific research in the field of liquid-liquid extraction purification of diesel distillates differing in the content of undesirable aromatic and sulfur compounds using various ionic liquids as a selective, environmentally friendly solvent are presented. Different extracting ability of ionic liquids (dipropylammonium, dibutylammonium and N-methylpyrrolidinium acetate, morpholinium formate) in relation to the extracted components of diesel distillate is shown. In particular, a high degree of purification of the hydrotreated diesel fraction was established when using N-methylpyrrolidinium acetate ionic liquid in the extraction process. The influence of the staged process of extraction purification of mixed diesel distillate based on straight-run diesel fraction (70% vol.) and secondary oil processing products - light gas oil coking and light gas oil catalytic cracking (30% vol.) on the degree of dearomatization and desulfurization of the fuel has been determined. A relatively high yield and degree of purification of diesel fuel were revealed when carrying out the process of extraction purification of the mixed diesel distillate with N-methylpyrrolidinium acetate ionic liquid in three stages. The extraction purification process was studied using IR and UV spectral analysis methods and the possibility of purifying three- and fourcyclic aromatic hydrocarbons from the mixture of straight-run diesel fraction and secondary petroleum products was established when carrying out the extraction process with N-methylpyrrolidinium acetate ionic liquid. [ABSTRACT FROM AUTHOR]

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In this study, a method for separating isopropanol from wastewater using hydrophobic deep eutectic solvents (DESs) synthesized from terpenes and capric acid was proposed. The distribution coefficient and selectivity value of isopropanol (IPA) in the solvents were determined by liquid–liquid extraction experiments, and the extraction performances of the solvents at different molar ratios and temperatures were studied. From the perspective of molecular dynamics simulations, the experimental results were verified by mechanism analysis, the contribution of hydrogen bond donors (HBDs) and hydrogen bond acceptors (HBAs) to the selective separation of isopropanol was explained. The interaction energies, radial distribution functions, normal density distribution, and mean square deviations between the atoms were used to analyze the interactions between the components of the DESs and IPA/water. It was observed that the DESs have a good extraction effect on IPA, which verifies the good application prospects of DESs in wastewater solutions containing alcohol compounds. [ABSTRACT FROM AUTHOR]

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

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

Liquid–liquid extraction is one of the most scalable processes to produce rare-earth elements (REEs) from natural and recycled resources. Accelerating the research, development, and deployment (RD&D) of sustainable processes to manufacture REEs requires both facile synthesis of extractive ligands at scale and fast evaluation of process conditions. Here, we establish an integrated RD&D methodology comprised of agile ligand synthesis and automated high-throughput extraction studies. Using diglycolamides (DGAs) as an example, we first developed a method for DGA synthesis (scalable to 200 g) by directly coupling diglycolic acid and secondary amines via the solvent-free melt-amidation reaction. A substrate scope of the melt-amidation synthesis was demonstrated for 9 different DGAs with good yields (85–96%) and purities (88–96%) without any post-reaction workup or purification process. Life cycle assessment shows that our synthesis method outperforms the prior-art pathway in each environmental impact category, especially showing a 67% reduction in global warming potential. Furthermore, we investigate the structure–activity relationship of various alkyl-substituted DGAs using an automated, high-throughput workflow for liquid–liquid extraction, achieving over 180 runs in 48 hours. The acquired data enables the development of a promising flowsheet for separating light and heavy REEs. The integrated RD&D method of agile synthesis and automated, high-throughput extraction studies paves the way for future iterative development of sustainable production of REEs and other critical materials to meet the needs for clean energy transformation. [ABSTRACT FROM AUTHOR]

Rationale: Accurate identification of old rice samples from new ones benefits their market circulation and consumers. However, the current detection methods are still not satisfactory because of their insufficient accuracy or (and) time‐consuming process. Methods: Chelating carboxylic acids (CCAs) were selectively extracted from rice, by stirring with chelating resin and a dilute Na2CO3 solution. The green analytical chemistry guidelines for sample preparation were investigated by using the green chemistry calculator AGREE prep. The extractant was determined by liquid chromatography–mass spectrometry (LC/MS), and statistical analysis of the analytical data was carried out to evaluate the significance of the difference by ChiPlot. Results: The limit of quantitation for the CCAs is in the range of 1 to 50 ng/mL, with a reasonable reproducibility. The CCAs in 23 rice samples were determined within a wide concentration range from 0.03 to 1174 μg/g. Intriguingly, the content of citric acid, malonic acid, α‐ketoglutaric acid and cis‐aconite acid in new rice was each found to be distinctively higher than that in old rice by several times. Even mixtures of old and new rice were found to show much difference in the concentration of citric acid and malic acid. Conclusion: A green analytical method has been developed for the simultaneous determination of CCAs by LC/MS analysis, and the identification of old rice samples from new ones was easily carried out according to their CCA content for the first time. The results indicated that the described method has powerful potential for the accurate identification of old rice samples from new ones. [ABSTRACT FROM AUTHOR]

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

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

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

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

Honey bee venom (HBV) is a valuable bee product famous for its therapeutic efficacy. HBV has a complex matrix containing several compounds, of which melittin is identified as the major component and can be considered an indicator compound. According to the numerous pharmacological effects of HBV, it can be a great candidate as an efficient active pharmaceutical ingredient (API). Despite the widespread analysis of crude HBV, not enough evaluations have been conducted on HBV pharmaceutical products, which is crucial in quality control procedures. Following the importance of APIs assay, we aimed to develop a feasible and valid HBV extraction method from cosmeceutical creams using precipitation techniques, and an analysis method was developed and validated based on high‐performance liquid chromatography. The analysis was well performed with a high separation capability. The method was repeatable and accurate and exhibited a linear behavior in melittin's 0.1–1.4 mg/mL concentration range. Accordingly, the extraction method revealed a notable recovery between 86% and 104%, and a 0.007 mg/mL detection limit and 0.022 mg/mL limit of quantification were estimated, respectively. Consequently, both extraction and analysis methods were considered valid and feasible, which may influence the quality control tests of HBV pharmaceutical and cosmetic products. [ABSTRACT FROM AUTHOR]

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

Two Hyptis plants endemic to Taiwan, H. rhomboides and H. suaveolens, contained xanthine oxidase inhibitors. To chemically investigate more herbs of the same genus, this study aimed to explore bioactive constituents from Hyptis spicigera leaf and the aerial part of H. brevipes, which would also enrich the chemotaxonomic basis for the Hyptis plants. The EtOH extract of the plant materials was fractionated by liquid‐liquid partitioning, followed by separation over various chromatography. High‐performance liquid chromatography‐solid phase extraction‐nuclear magnetic resonance hyphenation, a sustainable and environmentally friendly instrument, was applied to accelerate the chemical investigation of each subfraction. Eighteen isolates from Hyptis spicigera leaf and 14 compounds from H. brevipes aerial part were characterized. Of these, 12 compounds are rosmarinic acid derivatives, of which 9′‐O‐methyl melitrate A (10) and sagecoumarin methyl ester (22) are tentatively identified as new compounds. In total, 25 compounds were separated and characterized from Hyptis spicigera leaf and H. brevipes aerial part. Of these, seven of them (2–4, 11, 12, 18, 20) are in common between these two species, and 17 isolates (2–4, 8‐14, 22, 23, and 26‐30) are phenylpropanoids which are commonly distributed in the Labiatae family. [ABSTRACT FROM AUTHOR]

A fully continuous-flow nitration and post-processing protocol has been introduced into the preparation of 4-nitropyrazole. The process started from the nitration reaction of pyrazole with mixed acid, followed by continuous quenching, neutralization, extraction and separation. After the collected organic phase was rotationally evaporated to recover the solvent, the final product 4-nitropyrazole was obtained with 96.9% yield, 99.3% purity and 381 g/h productivity. By establishing a kinetics model and MATLAB simulation calculation, it worked out to achieve the preferable selectivity conditions of mono-nitration product 4-nitropyrazole. The process of post-processing solved the problems of solid precipitation and extractant hydrolysis. The extraction process was determined by the distribution coefficient and twice extraction was used to reduce the amount of organic solvent. [ABSTRACT FROM AUTHOR]

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

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

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

Introduction: Thyroid cancer incidence rate has increased substantially worldwide in recent years. Fine needle aspiration biopsy (FNAB) is currently the golden standard of thyroid cancer diagnosis, which however, is invasive and costly. In contrast, breath analysis is a non-invasive, safe and simple sampling method combined with a promising metabolomics approach, which is suitable for early cancer diagnosis in high volume population. Objectives: This study aims to achieve a more comprehensive and definitive exhaled breath metabolism profile in papillary thyroid cancer patients (PTCs). Methods: We studied both end-tidal and mixed expiratory breath, solid-phase microextraction gas chromatography coupled with high resolution mass spectrometry (SPME-GC-HRMS) was used to analyze the breath samples. Multivariate combined univariate analysis was applied to identify potential breath biomarkers. Results: The biomarkers identified in end-tidal and mixed expiratory breath mainly included alkanes, olefins, enols, enones, esters, aromatic compounds, and fluorine and chlorine containing organic compounds. The area under the curve (AUC) values of combined biomarkers were 0.974 (sensitivity: 96.1%, specificity: 90.2%) and 0.909 (sensitivity: 98.0%, specificity: 74.5%), respectively, for the end-tidal and mixed expiratory breath, indicating of reliability of the sampling and analysis method Conclusion: This work not only successfully established a standard metabolomic approach for early diagnosis of PTC, but also revealed the necessity of using both the two breath types for comprehensive analysis of the biomarkers. [ABSTRACT FROM AUTHOR]