This study synthesized magnetic biochar derived from oil palm fronds (M-OPFAC) to extract four organochlorine pesticides (OCPs) from tea using magnetic solid-phase extraction (MSPE). The extracted substances were then quantified with gas chromatography-mass spectrometry (GC-MS). This study also employed a conductor-like screening model for real solvents (COSMO-RS) to predict the dominant intermolecular interactions involved. Furthermore, Fourier transform infrared spectroscopy (FTIR), field-emission scanning electron microscopy (FESEM), Brunauer-Emmett-Teller (BET) analysis, N-2 adsorption-desorption isotherm and vibrating sample magnetometer (VSM) were used to thoroughly characterize the synthesized sorbent, including its functional groups, morphology, surface area, and magnetic properties. The Plackett-Burman design was employed to screen primary extraction variables, while optimization of significant factors using the Box-Behnken design (p < 0.05) yielded the final conditions: 30 mg sorbent, 19 mL sample volume, and 1.1 mL desorption solvent. Resultantly, excellent linearity (10-500 mu g/L) and low detection limits (0.052-0.091 mu g/L) were attained with 30 mg sorbent and 1.0 mL desorption solvent. Analysis of real and spiked tea samples also yielded 89.1% to 102.7% recovery, with relative standard deviations (RSDs) below 5%, and allowed for three regeneration cycles. Meanwhile, the COSMO-RS analysis confirmed van der Waals forces as the primary adsorption mechanism.

ABSTRACT Medicago sativa L. (alfalfa) harbors a remarkably diverse reservoir of bioactive secondary metabolites. Flavonoids, isoflavones, and triterpenoid saponins dominate its bioactivity landscape, driving potent antioxidant, anti‐inflammatory, antimicrobial, estrogenic, hypolipidemic, and cytotoxic actions through redox modulation, membrane perturbation, receptor engagement, and suppression of NF‐κB/MAPK signaling. Evidence converges on multi‐organ protection, improved endothelial tone and lipid profiles, neuroprotection via oxidative‐stress quenching, photoprotection afforded by carotenoids and flavones, and selective antitumor effects through apoptosis induction and cell‐cycle arrest. Emerging research applications, of M. sativa L. saponins include functional‐food fortification, bio‐emulsifier applications and sustainable crop‐protection strategies. Despite these promising insights, heterogeneity in extraction protocols, lack of phytochemical standardization, and scarce pharmacokinetic or long‐term safety data currently affect M. sativa L. usage. This systematic review provides a comprehensive compound‐by‐compound matrix linking chemical classes to their biological functions, thereby establishing a reproducible platform for targeted metabolomic, toxicological, and controlled trial investigations aimed at unlocking the biomedical and biotechnological potential of M. sativa L. phytochemicals. The novelty of this work lies in its systematic integration of all currently available phytochemicals reported in alfalfa, together with their nutraceutical and functional food implications, which extends beyond the scope of earlier reviews. By highlighting structure–activity trends and pinpointing unexplored mechanistic nodes, this review aims to accelerate M. sativa L. nutraceutical design and regulatory appraisal worldwide.

Medicago sativa L. (alfalfa) is increasingly recognized as a rich source of health-promoting phytochemicals whose efficient, sustainable recovery remains technically challenging. This systematic review revises current extraction strategies and associated bioactive profiles, providing an evidence-based roadmap to obtain extracts valuable for the food, nutraceutical and pharmaceutical sectors. A PRISMA-guided search of PubMed, Scopus and Web of Science (literature up to March 2025) yielded 80 eligible studies. These investigations collectively report 124 distinct bioactive constituents—classified into 13 chemotypes (alkaloids, amino-acid derivatives, carbohydrates, carotenoids, coumarins, coumestans, flavonoids, phenolics, pigments, saponins, sterols, terpenoids and vitamins)—isolated from alfalfa leaves, stems, roots or seeds. Extraction technologies were grouped as conventional (maceration, Soxhlet, hydrodistillation) or innovative (ultrasound-, microwave-, enzyme-, pulsed-electric-field and supercritical-fluid-assisted methods). Meta-comparison shows that innovative technologies—particularly ultrasound-assisted extraction, supercritical CO₂ (with ethanol as co-solvent) achieves equal or superior yields of key flavonoids, phenolics and triterpene saponins while reducing solvent consumption (30–90 %), energy use (40–70 %) and thermal degradation relative to conventional techniques.

Oil spills are among the most serious environmental pollutants affecting aquatic ecosystems. In this study, a superhydrophobic magnetic graphene (MG) adsorbent was synthesized and applied for crude oil removal from aqueous solutions. The effects of pH, salinity, adsorbent dosage, temperature, and contact time were optimized. Under the optimum conditions (pH 10, salinity 4.1

This study presents the development and application of a thermally reduced graphene (TRG)-modified SiO2-APTES composite for the extraction and preconcentration of cadmium (Cd (II)) ions from aqueous samples, with quantification by UV-Vis spectrophotometry. To enhance the selectivity of Cd(II) detection, diphenylthiocarbazone (dithizone) was used as a chelating agent prior to the extraction process. Critical parameters, including the type and volume of the desorption solvent, pH, adsorbent dosage, and salt concentration, were systematically investigated and optimized. The optimized method achieved a preconcentration factor of 200 for a 30 mL sample volume. The method demonstrated excellent analytical performance, with a linear dynamic range of 1.0-100 ngmL-1, a determination coefficient (R2) of 0.995, a limit of detection (LOD) of 0.5 ngmL-1, and a relative standard deviation (RSD) of 4.1% at a Cd (II) concentration of 10 ngmL-1 (n = 3). Application to real water samples yielded relative recoveries (RR) of approximately 94%, confirming the method's reliability and robustness. This approach combines high sensitivity, cost-effectiveness, and operational simplicity, making it a promising tool for trace-level cadmium detection in environmental and water quality monitoring applications.

In this study, plain zeolite (ZSM5) and hierarchical zeolite (H-ZSM5) were synthesized as efficient adsorbents for the removal of polyphenolic/antioxidant compounds from olive mill wastewater (OMW). The XRD and FTIR results confirmed the successful synthesis of ZSM5 zeolites. SEM images and BET demonstrated that H-ZSM5 possessed a markedly greater surface area of 337.99 m(2)/g in contrast to ZSM5 (162.84 m(2)/g). For H-ZSM5, the values determined for pore volume, total volume, and pore diameters are 77.655 cm(3) g(-1), 0.1844 cm(3) g(-1), and 2.1826 nm. The absolute zeta potential values varied between 5.36 +/- 1.21 and - 46.41 +/- 1.32 mV, with the peak absolute value of - 46.41 +/- 1.32 mV occurring at pH 4. The optimal conditions for the removal of phenolic compounds, achieving an efficiency exceeding 90%, were identified as a pH of 4, an adsorbent dosage of 50 mg, and a contact duration of 90 minutes. The adsorption isotherm was found to align with the Langmuir model rather than the Freundlich model, indicating a monolayer adsorption capacity of 48.7 mg/g. Kinetic studies were consistent with a pseudo-first-order model (R-2 >0.99). Ultimately, the thermodynamic analysis suggested that the adsorption of OMW onto ZSM5 is both spontaneous and governed by a physisorption mechanism.

A new nanocomposite based on alginate microbeads impregnated with novel strontium-aluminum layered double hydroxide (Sr-Al LDH) incorporated with choline chloride-urea deep eutectic solvent (ChCl-U DES) was introduced. The microbeads and LDH were characterized by adsorption/desorption isotherms, Fourier-transform infrared spectroscopy, SEM, and x-ray diffraction. The adsorbent was employed for determining penicillin G (PENG) using dispersive solid-phase extraction prior to HPLC analysis. The extraction efficiency of the adsorbent, compared with that of unmodified alginate, showed a 2.5-fold increase. Significant parameters, including elution conditions, sorbent composition and mass, adsorption time, and sample pH, were optimized. The LOD was 0.4 µg kg-1, and the linear range was 1.4-500 µg kg-1. The LOQ (1.4 µg kg-1) was lower than the established maximum level for PENG by the European Union (4 µg kg-1). Enrichment factor and synthesis reproducibility were also investigated. The method's accuracy was evaluated through PENG analysis in dairy products and water, with recoveries of 81%-107% (RSDs < 7.6%). The procedure's greenness was assessed using the Analytical Eco-scale and achieved excellent green credentials. To the best of our knowledge, this is the first report on the synthesis and application of a novel alginate composite for the extraction of PENG from dairy and water samples.

In this study, sesame cake was valorized to produce sesame protein hydrolysate (SPH) with improved functional and antioxidant properties using a recoverable nanomagnetic immobilized Alcalase (ALC); the process was accelerated in the microreactor through a controlled-hydrolysis technique. For this purpose, silica-coated magnetic nanoparticles (Fe3O4@SiO2) were synthesized and functionalized with tetraethoxysilane (TEOS), N-(trimethoxysilylpropyl) ethylenediamine (TMSED), and finally activated with glutaraldehyde (GLU) to produce Fe3O4@SiO2-TMSED-GLU. Immobilization efficiency of ALC was 88.78 % in the optimum conditions of ALC concentration (1.23 mg/mL), immobilization period (119.12 min), and temperature (38.93 degrees C). The successful synthesis of Fe3O4@SiO2-TMSED-GLU-ALC magnetic nanobiocomposite (MNBC) was approved using FTIR, XRD, VSM, FESEM, EDX, and elemental mapping. The effective immobilisation of the enzyme was responsible for the decrease in the intensity of Fe3O4 diffraction peaks (in XRD) in MNBC and a reduction in saturation magnetization (in VSM) following ALC immobilisation. Microreactor-intensified hydrolysis in the optimized conditions of MNBC = 4.85 wt%, reaction time = 54.10 s, and temperature = 46.95 degrees C, led to a degree of hydrolysis = 7.19 %. After 10 hydrolysis cycles, MNBC had relative activity > 80 %, due to the appropriate covalent bonding between the enzyme and the support and the short duration of the process. The produced SPH had superior foaming capacity (113.09 %) compared to sesame protein (76.34 %). The emulsion activity and emulsion stability of SPH were 28.78 m(2)/g and 56.43 min, respectively, which were higher than those of the sesame protein.

Catechins, as powerful flavonoids with antioxidant properties, are crucial for the preservation of the human body against free radicals and for promoting overall health. Research has shown that the presence of catechins in urine is linked to a reduced risk of gastric and esophageal cancer. This study introduces an innovative approach using a novel nano-composite material, composed of magnetic graphene oxide coated with a biocompatible O-carboxymethyl chitosan/acrylic acid copolymer, for extracting catechins from human urine. The extracted catechins were then analyzed using gas chromatography/mass spectrometry-selected ion monitoring analysis. Under the optimum conditions, the analytical figures of merit for catechin and epicatechin were linear dynamic range: 0.5-1000 ng/mL, R2 of 0.9991; limit of detection equal to 0.1 ng/mL; relative standard deviation: 4.1 and 3.1 (C = 50 ng/mL, n = 3); and relative recovery was 94%, respectively. The application of this method holds significant promise for advancing clinical and toxicological studies, as well as establishing potential associations between tea consumption and disease prevention.

A novel nanocomposite based on bacterial cellulose (BC) modified by manganese sulfide (MnS) decorated graphene oxide (GO) was prepared. The hydrogel was characterized by Fourier transform infrared, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and adsorption/desorption techniques. The sorbent was employed for determining acrylamide in bread samples using micro-solid-phase extraction coupled with high-performance liquid chromatography. The extraction efficiency of prepared sorbent was 1.4-fold higher than that of BC. The important extraction factors including elution conditions (acetonitrile 300 mu L, 5 min), sorbent composition and mass (50 mg), adsorption time (7 min), sample solution pH (8), and salt effect (3% w/v) were considered for optimization of the method. The analytical merit was validated by assessing the preconcentration factor (178-225), limit of detection (1.56 mu g/kg), limit of quantification (5.15 mu g/kg), linearity (5.15-500 mu g/kg), and determination coefficient (0.9845). The adsorption isotherms and kinetic studies demonstrated that the adsorption process followed the Langmuir model and pseudo-second-order kinetics. The relative recoveries and relative standard deviations were 84%-106% and 2.4%-9.2%, respectively. This paper is the first report on the fabrication and use of BC doped with MnS-GO composite for extraction of acrylamide in typical commercial bread samples.

Background: Common solvents are mainly volatile organic compounds derived from petroleum, which are harmful to human health and the environment. Reducing the consumption of these toxic solvents or replacing them with safe solvents is vital. Recently, it has suggested the use of green alternative solvents as a proper solution. Scope and approach: The present study reviews various aspects of amino acid-based natural deep eutectic solvents (AABNADESs) from synthesis to application. This investigation can provide a theoretical basis for the extensive application of AABNADESs in extraction of various analytes and also can be a guidance to choose the proper solvent for each analyte. Key findings and conclusions: Amino acid-based deep eutectic solvents are natural plant metabolites with at least one amino acid component that can be synthesized in various physical ways through the formation of hydrogen bonds. These emerging and green solvents are competitive to organic solvents to recover a wide range of analytes and can be a suitable alternative to toxic solvents in the field of extraction due to reasons such as biodegradability, tunable features, and being safe. Adjusting the inherent characteristics of DESs and optimizing other factors are necessary in order to achieve the highest extraction efficiency.

The catalytic activity of the lanthanum nickelate (LaNiO3; LNO) and cobalt-doped lanthanum nickel oxide (LaNi1-xCoxO3; LN1-xCxO) as Ni-based perovskite structures for the waste vegetable cooking oil (WVCO) conversion to biodiesel was assessed. The phase purity and structural identity of the synthesized samples LNO and LN1-xCxO were verified by BET, NH3/CO2-TPD, SEM-EDX, ICP-OES, XRD, and TEM. From analyzing the characterization of catalysts, it is evident that doping LNO with cobalt, in addition to increasing the catalyst's surface area, by the formation of oxygen vacancies in the perovskite structure caused the improvement of the catalytic activity by providing more active sites during the WVCO transesterification reaction. According to the analysis of the data obtained from the optimization of the WVCO transesterification reaction via response surface methodology (RSM) based on the central composite design (CCD), the use of the LN0.8C0.2O catalyst resulted in the WVCO conversion of 97.28% to biodiesel.

The potential decline in crude oil reserves and rising awareness of the detrimental environmental impacts of consuming fossil fuels promoted the creation of alternative approaches to transform waste biomass into biofuels. This research provided a simple approach for synthesizing barium tin oxide (BTO) and its decoration over the reduced graphene oxide (RGrO) to manufacture BTO@RGrO as an efficient catalyst in the process of biodiesel production from waste cooking oil (WCO). The prepared BTO and BTO@RGrO nanocomposite were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Energy-Dispersive X-ray Spectroscopy (EDX), BET (Brunauer, Emmett, and Teller), Temperature Programmed Desorption of NH3/ CO2 (NH3/CO2- TPD), and Power X-ray diffraction (XRD). The response surface methodology (RSM) based central composition designs (CCD) was employed to optimize the influence factors, including reaction temperature (40-90 degrees C), reaction duration (10-50 min), catalyst quantity (1-5 wt%), and methanol to oil (MeOH/Oil) molar ratio (5-25). The optimal performance of biodiesel generated was acquired over BTO@RGrO nanocomposite at the reaction temperature of 68.83 degrees C, reaction duration of 27.95 min, catalyst quantity of 3.21% by weight, and MeOH/Oil molar ratio of 14.93, which led to biodiesel generation with a 97.03% purity. The finding revealed that the BTO@RGrO nanocomposite could be effectively utilized as a stable heterogeneous solid catalyst under ideal reaction conditions with outstanding catalytic performance.

This study investigated the physicochemical properties and polyphenol composition of extra virgin olive oils (EVOOs) extracted from three olive cultivars. The investigated cultivars were Arbequina, Koroneiki, and Manzanilla, grown in Olive Research Station in Rudbar county, Gilan province, Iran, at three ripening stages. Several parameters were analyzed, including peroxide and acidity values, unsaponifiable matter, oxidative stability, total aliphatic alcohols, fatty acids (FAs), sterols, and triacylglycerol composition. The results showed that as maturity increased, parameters such as oil content, acidity value, and iodine value, rise, while parameters including peroxide value, oxidative stability, aliphatic alcohols, and unsaponifiable matter decreased (p < .05). The saponification value was slightly reduced in the developing ripening process (p > .05). The MUFA/PUFA ratio and total sterol content declined during the olive ripening stages (p < .05). The triterpenes decreased in Arbequina and Koroneiki cultivars but increased in Manzanilla cultivar during the maturity stages. According to the data, oleuropein decreased while oleuropein aglycone, oxidized aldehyde, and hydroxylic form of oleuropein increased for all EVOOs during maturation. Apigenin, quercetin, ligstroside aglycone, aldehyde and hydroxylic form, ferulic acid, caffeic acid, and catechin decreased during the ripening of fruits (p < .05). The main triglycerides were triolein (OOO), palmitodiolein (POO), dioleolinolein (OOL), and palmitooleolinolein (PLO) in all EVOOs. In addition, the olive cultivar and harvesting date influence the physicochemical properties and polyphenol composition of EVOOs extracted from olive varieties grown in one region. In conclusion, the results can present helpful information to determine the optimum maturity stage for the investigated olive cultivars.

In the present study, a magnetic nano gel as the sorbent which is the combination of octatonic acid: cumarin as eutectic solvent and Fe3O4@SiO2 was introduced as the sorbent in ultrasound-assisted dispersive µ-solid phase extraction process coupled with high performance liquid chromatography with photo diode array detector for simultaneous separation and determination of tetracyclines residues in food samples. FT-IR, SEM, VSM were used for the characterization of the synthetized magnetic nano gel. Under obtained optimum conditions, the obtained linear ranges were 1.5–500 (µg L−1), 2.5–750 (µg L−1), 2–750 (µg L−1), and 2.5–500 (µg L−1) for tetracycline, oxytetracycline, chlortetracycline, and doxycycline, respectively. Moreover, the below level of quantification (BLQ) (based on S/N = 3) of 0.47 µg L−1, 0.11 µg L−1, 0.85 µg L−1, 0.66 µg L−1, 0.81 µg L−1 and the limit of quantification (based on S/N = 10) of 1.61, 2.74, 2.23 (µg L−1), and 2.66 were achieved for tetracycline, oxytetracycline, chlortetracycline, and doxycycline, respectively. The intra-day and inter-day precision (

A green dispersive liquid-liquid microextraction procedure based on a ternary polymeric hydrophobic deep eutectic solvent (DES) for monitoring multi-residue pesticides in eleven various fruit juices was developed before Gas Chromatography coupled with micro-Electron Capture Detector (GC-& mu;ECD). Six ternary polyethylene glycol (PEG)-based DESs were synthesized, and their extraction efficiency was evaluated. Among these DESs, [thymol]: [polyethylene glycol]:[acetic acid] (1:2:2) showed the highest signal intensity. Moreover, three other binary PEG-based DESs and a non-polymeric DES were also synthesized and compared to the previous DES. The extraction yield obtained by polymeric one was much higher than non-polymeric. Some significant parameters influencing the extraction efficiency including the type and volume of DES (extraction solvent), disperser solvent, pH, and ionic strength were optimized as follows: [Thy]:[PEG]:[HOAc] (1:2:2), 400 & mu;L of DES, ACN as disperser solvent (700 & mu;L), no pH adjustment and no salt addition. The DES was characterized by ATR-FTIR and (1H and 13C) NMR spectroscopy. Under the optimized conditions, the limits of quantification, the linear ranges and extraction recovery were 0.009-0.182 & mu;gL-1 0.003-50.0 & mu;gL-1, 67.9-108.4%, respectively. The enrichment factors were 11-170. Intra-day and inter-day RSDs% were 1.4-5.1% and 2.0-12.6%, respectively. This method was applied for analyzing pesticide residues in eleven fruit juices, and the pre-concentration factor and relative extraction recoveries were in the range of 12-169 and 71-108%, respectively.

Antioxidant properties of essential oils (EOs) depend on environmental, genetic and other factors. We hypothesized that the EOs of rosemary (Rosmarinus officinalis), lavender (Lavendula sublepoidota) and Ferulago contracta may be affected by distillation methods. This study investigated the effects of hydrodistillation (HD) and steam distillation (SD) on bioactive compounds yield, total phenol content (TPC), total flavonoid content (TFC), and antioxidant property of rosemary, lavender and F. contracta EOs. Results showed that the yield of EO in SD was significantly higher than HD (p < 0.05). Thumbnail (11.28

This research used titanium oxide-coated magnetic Fe3O4 nanoparticles doped graphene oxide (MTiGO) and modified with Candida antarctica Lipase B (CALB) enzyme. The MTiGO@CALB nanocomposite is a novel biocatalyst for transesterifying triglycerides to fatty acid methyl esters (FAMEs) from waste cooking oil. tThe physicochemical characteristics of the proposed biocatalyst were determined via FTIR, VSM, XRD, SEM, and EDS techniques. The maximum immobilization efficiencies and activity recovery of immobilized enzymes were obtained at 89% and 75% in the following operating condition: lipase concentration of 2.0 mg/mL, pH of 7.0, immobilization temperature of 35 degrees C, and immobilization time of 4 h. Various effective parameters on biodiesel were stated, and according to the revealed data, the maximum yield of biodiesel via the transesterification process was achieved at 92%, at a reaction temperature of 45 degrees C, catalyst quantity of 4 wt%, aa reaction duration of 40 h, and methanol to molar oil ratio of 5:1 These findings indicated that the provided bio-nanocomposite has a high potential for producing biodiesel as an efficient heterogeneous biocatalyst.

The conditions of production of multiple W/O/W nanoemulsions containing sesamol and retinol were optimized using response surface methodology (RSM). Span 80 (5, 10, and 15 % w/v), Tween 80 (1, 5.5, and 10 % w/v), and water in oil ratio (W/O) (20, 30, and 40 %) were considered as independent variables while encapsulation efficiency (EE%) and particle size were taken as dependent variables. Alginate (Alg) and chitosan (CS) were also applied to form a deposit layer. An optimum sample with an EE of 92.93 % and particle size of 381.94 nm was produced when Tween 80, Span 80, and W/O were 6.24 %, 10.84 %, and 37.70 %, respectively. Based on the Fourier transform infrared spectroscopy (FTIR), detection of hydrophobic band (2899 cm-1) approved the physical entrapment of biomolecules. Differential scanning calorimetry (DSC) indicated an endothermic peak at 236.48 °C associated with the ionic interactions of Alg-CS. Confocal laser scanning microscopy (CLSM) indicated Alg-CS complex deposit layer formed by electrostatic attraction surrounding the W/O/W multiple layers. The in vitro release of sesamol and retinol was 39 % of sesamol and 22 % of retinol in simulated gastric fluid (SGF) and 56 % and 22 % in simulated intestinal fluid (SIF), respectively.

Pesticides are a large group of pristine organic contaminants, which are widely discharged into environmental water due to agricultural activities. Hence, extraction, determination, and removal of pesticides from water resources are necessary for human health. In this study, novel adsorbent was developed based on three-dimensional magnetic graphene coated with gold nanoparticles (3D-MG@AuNPs) for extraction of chlorpyrifos, dicrotophos, fenitrothion, and piperophos as four specific organophosphorus pesticides (OPPs) from wastewater and tap water samples. The proposed nanocomposite was characterized; FTIR and EDX are performed for the expected functional groups and elemental analysis, SEM showed the unique and spherical AuNPs are well dispersed over graphene sheets. In this investigation, the important parameters that have effect on the extraction efficiency, including the desorbing solvent, desorbing solvent volume, vortex time, the extraction time, adsorbent dosage, pH of sample solutions, and salt effect were evaluated. In conclusion, the measured amounts of the chosen OPPs were determined using the gas chromatography microelectron capture (μECD-GC) method. Limits of quantification (S/N ratio of 10) and detection (S/N ratio of 3) were attained at concentrations of 0.26-0.43 μg.L-1 and 0.08-0.14 μg.L-1, respectively. According to the results of the investigations, the synthesized 3D-MG@AuNPs did not require any complicated sample preparation methods; therefore, it is a very good choice for solid magnetic phase extraction studies.