Optimal Extraction Conditions Research Articles

Extraction of rhodium from supported liquid-phase hydroformylation catalysts with supercritical carbon dioxide

The continuous extraction of the rhodium inventory in supported liquid-phase (SLP) catalytic materials utilized in the hydroformylation (HyFo) of 1-butene was investigated by supercritical carbon dioxide (scCO2). Optimization of extraction efficiency involved varying parameters such as temperature (90 and 120 °C), pressure (10, 20 and 30 MPa), and the addition of methanol as a polar co-feed to the extraction medium (0–20 vol%). The results underscored the critical role of methanol in facilitating extraction, as experiments employing pure scCO2 yielded no rhodium recovery. Furthermore, extraction performance demonstrated sensitivity to temperature and pressure adjustments during the process. Notably, the use of 10 vol% methanol at 120 °C and 30 MPa achieved complete rhodium extraction from the grained SLP materials, which was identified as the optimum extraction condition. This study highlights the potential for scaling up in-situ rhodium extraction processes within HyFo production plants based on SLP catalysts, emphasizing significant implications for industrial applications.

Simultaneous determination of ethylene oxide, 2-chloroethanol and ethylene glycol residues in medical device products by gas chromatography

A gas chromatography-based method was developed for the simultaneous and rapid determination of ethylene oxide (EO), 2-chloroethanol (ECH), and ethylene glycol (EG) residues in medical devices after EO sterilization. A sample weighing 2.5 g was added with 5 mL of ethanol as the extraction medium, and the residual substances in the sample were extracted at 40 ℃ for 4 h. The samples were separated on a DB-WAX capillary column (30 m×0.53 mm×1.0 μm) and determined using a hydrogen flame ionization detector. The temperature was maintained at 40 ℃ for 5 min, increased to 120 ℃ at a rate of 40 ℃/min, held for 5 min, and then increased to 200 ℃ at a rate of 6 ℃/min, held for 2 min. The flow rate of the nitrogen gas was 3 mL/min. The split ratio was 5∶1. The inlet and detector temperatures were 200 and 300 ℃, respectively. The changes in the chromatographic peak areas over time (0.5-10 h) under different temperatures (20, 30, 40, and 50 ℃) were investigated, and the optimal extraction condition was determined to be 40 ℃ for 4 h. In the experiments, quantification was performed using an external standard method. EO, ECH, and EG exhibited good peak shapes and separation effects as well as good linearity within their respective ranges. The linear correlation coefficients for EO, ECH, and EG were greater than 0.99. The limits of detection (LODs) for EO, ECH, and EG were in the range of 0.10-0.40 μg/g, and the limits of quantification (LOQs) were in the range of 0.30-1.20 μg/g. The average recoveries under different spiked levels were in the range of 91.08%-116.08%, and the relative standard deviations (n=6) were in the range of 0.56%-8.45%. EO, ECH, and EG residues were found to exist at different levels in the medical devices tested. In particular, disposable infusion sets must be paid careful attention. ECH and EG were not detected in disposable sterile medical devices made of non-polyvinyl chloride materials, which may be due to the fact that the products themselves did not contain chloride ions, they were not exposed to chlorine-containing substances during their production, sterilization, storage, transportation, use, etc. This study established a method to detect EO residues in disposable medical devices, and has the advantages of simple operation, excellent specificity, accurate quantification, and good reproducibility. It can simultaneously detect three residual substances in medical devices while meeting the actual detection requirements for EO, ECH, and EG residues. The method can be used to scientifically and effectively evaluate the risk of EO residues in single-use medical devices sterilized with EO, and will be helpful for improving the quality of medical devices, ensuring the safety of device use, and providing a reference for regulatory supervision and testing.

Extraction of mucilage polysaccharides from chia seed by hydrophobic deep eutectic solvents-based three-phase partitioning system: A phase behavior-driven approach

By incorporating the hydrophobic deep eutectic solvents (DESs) into the three-phase partitioning (TPP) technique, a TPP-based method was developed to extract the chia seed polysaccharide (CSP) from chia seed. Through a single-factor experiment and response-surface model, the optimal condition for the TPP extraction was determined as DES composed of dodecanoic acid and octanoic acid in a 1:1 M ratio, (NH4)2SO4 concentration of 32.86 %, crude extract–DES ratio of 0.93 (v/v), aqueous phase pH of 4.38, extraction temperature of 35 °C, and extraction time of 10 min. The polysaccharide yield of the constructed TPP method is 8.65 %, which is higher than the conventional water extraction method (yield is 6.96 %). Molecular dynamics simulations reveal the phase behavior of proteins and polysaccharides in the TPP system, showing that noncovalent interactions play a crucial role in the TPP system. The CSP obtained by the TPP method exhibits distinctive composition, structural, physicochemical, and functional properties, leading to improved thermal stability, rheological behavior, and antioxidant performance. Compared with the traditional extraction method, efficient extraction of CSP can be achieved flexibly using the proposed TPP approach, resulting in high yield and quality of CSP, which provides a new path for the large-scale utilization of chia seed.

Biological activities of Hypericum spectabile extract optimized using artificial neural network combined with genetic algorithm application

Optimizing extraction conditions can help maximize the efficiency and yield of the extraction process while minimizing negative impacts on the environment and human health. For the purpose of the current study, an artificial neural network (ANN) combined with a genetic algorithm (GA) was utilized for that the extraction conditions of Hypericum spectabile were optimized. In this particular investigation, the main objective was to get the highest possible levels of total antioxidant status (TAS) for the extracts that were obtained. In addition to this, conditions of the extract that exhibited the maximum activity have been determined and the biological activity of the extract that was obtained under these conditions was analyzed. TAS values were obtained from extracts obtained using extraction temperatures of 30–60 °C, extraction times of 4–10 h, and extract concentrations of 0.25-2 mg/mL. The best model selected from the established ANN models had a mean absolute percentage error (MAPE) value of 0.643%, a mean squared error (MSE) value of 0.004, and a correlation coefficient (R) value of 0.996, respectively. The genetic algorithm proposed optimal extraction conditions of an extraction temperature of 59.391 °C, an extraction time of 8.841 h, and an extraction concentration of 1.951 mg/mL. It was concluded that the integration of ANN-GA can successfully be used to optimize extraction parameters of Hypericum spectabile. The total antioxidant value of the extract obtained under optimum conditions was determined as 9.306 ± 0.080 mmol/L, total oxidant value as 13.065 ± 0.112 µmol/L, oxidative stress index as 0.140 ± 0.001. Total phenolic content (TPC) was 109.34 ± 1.29 mg/g, total flavonoid content (TFC) was measured as 148.34 ± 1.48 mg/g. Anti-AChE value was determined as 30.68 ± 0.77 µg/mL, anti-BChE value was determined as 41.30 ± 0.48 µg/mL. It was also observed that the extract exhibited strong antiproliferative activities depending on the increase in concentration. As a result of LC-MS/MS analysis of the extract produced under optimum conditions in terms of phenolic content. The presence of fumaric, gallic, protocatechuic, 4-hydroxybenzoic, caffeic, 2-hydoxycinamic acids, quercetin and kaempferol was detected. As a result, it was determined that the H. spectabile extract produced under optimum conditions had significant effects in terms of biological activity.

Valorization of Potato Peels (Solanum tuberosum) Using Infrared-Assisted Extraction: A Novel Sprouting Suppressant and Antibacterial Agent

Recently, there has been a growing interest in reducing waste to promote environmental sustainability, with particular focus on agricultural by-products, especially fruits and vegetables. Potato, a widely used crop across various industries, generates a significant amount of peel waste. This study aims to valorize potato peels using water bath extraction (WBE) and infrared-assisted extraction (IRAE), both with distilled water as the solvent, followed by assessments of antioxidant, antibacterial, and anti-sprouting activities. Optimization using response surface methodology identified optimal extraction conditions for WBE (90 °C for 70 min) and IRAE (80 °C for 10 min), with both methods yielding 3.5 mg GAE/g DM in polyphenol content. IRAE demonstrated superior energy efficiency and enhanced antioxidant activity. The extracts exhibited antibacterial properties against both Gram-positive (Listeria monocytogenes) and Gram-negative bacteria (Proteus sp. and Salmonella sp.), with inhibition zones ranging from 10 to 14 mm. Furthermore, the potato peels extract showed significant anti-sprouting effects at room temperature, reducing both the number and size of sprouts compared with the control. HPLC analysis showed the presence of different phenolic compounds such as rutin, catechin, caffeic acid, protocatechuic acid, chlorogenic acid, p-coumaric acid, and gallic acid in one or both extracts. These findings suggest that potato peels extract holds potential for applications in the food industry as a natural preservative due to its antioxidant properties, as well as a sprout suppressant. The antibacterial activity of the extracts suggests their potential as a natural preservative as well, offering protection against both Gram-positive and Gram-negative bacteria that may be present in food.

Bio-Guided Extraction of a Phenolic-Rich Extract from Industrial Peanut Skin with Antioxidant and Hypotensive Potential

Peanut composition includes phenolic compounds, especially in the skins, which are often not consumed. High blood pressure affects more than one billion people worldwide and is considered a high-risk factor for cardiovascular diseases. Several studies have correlated antihypertensive activity with the total phenolic content present in the plants. This study evaluated the hydroethanolic extraction of phenolic compounds from the industrial residue of peanut skin and evaluated the antioxidant and antihypertensive capacity of these extracts using in vitro models. A rotational central composite design (DCCR) was proposed to study the influence of the variables: (1) the ethanol concentration on the hydroalcoholic extractor solution, and (2) the proportion of solid sample (waste) per liquid in the extraction (mass/volume) in a simple solid—a liquid extraction process. The optimal extraction conditions within this model were 50% ethanol in water, and the proportion of sample to extraction solution (m/v) equaled to 0.2. The extract obtained had significant antioxidant capacity, both in chemical (ORAC) and in cellular models, with potential for free radical scavenging. Significant levels of ACE inhibition were also found, indicating antihypertensive activity.

Ultra-high pressure assisted extraction of water-soluble polysaccharides from Moringa oleifera seed husks and their antioxidant activities

ABSTRACT The process conditions and antioxidant activity of ultra-high pressure assisted extraction of polysaccharides from Moringa oleifera seed husks were studied. Taking the yield of polysaccharides as the index, the effects of degree of crushing, extraction pressure, holding pressure time and material-to-liquid ratio on the yield of polysaccharides from Moringa oleifera seed husks were investigated. The optimal extraction conditions were determined by single-factor test and orthogonal test: a holding time of 10 min, a material-to-liquid ratio of 1:25, an extraction pressure of 350 MPa, and a polysaccharide yield of 0.264%. Its antioxidant activity can be determined by measuring the total antioxidant capacity and their ability to scavenge DPPH and ·OH radicals. The results showed that the IC50 of Moringa oleifera seed husk polysaccharides on DPPH and hydroxyl radicals were 0.0662 g/L and 0.0844 g/L, respectively. The total antioxidant capacity was 0.1826 mm/g (expressed as the equivalent concentration of ferrous sulfate). Compared with hot water extraction methods, ultra-high pressure assisted extraction methods can shorten extraction time, improve extraction efficiency. The water-soluble polysaccharides extracted from Moringa oleifera seed husks by ultra-high pressure assisted extraction technology also have higher antioxidant activity than that by hot water extraction method at the same concentration.

Comprehensive Study of Sustainable Pressurized Liquid Extractions to Obtain Bioavailable Antioxidant Phenolic Compounds from Grape Seed By-Products

Few investigations have been conducted to evaluate pressurized liquid extraction (PLE) technology as a sustainable method for the recovery of phenolic compounds of grape seed by-products. In this study, PLE combined with an experimental design was evaluated for optimizing the sustainable extraction of phenolic compounds from grape seed by-products. The solvent ethanol content (X1, 0–100%), temperature (X2, 20–100 °C) and time (X3, 1–11 min) were studied as independent experimental factors. Yield, TPC, antioxidant activity and phenolic composition were analyzed as optimized dependent variables. Two optimal extraction conditions at different temperatures (20 °C and 100 °C) were found, but thermal degradations at 100 °C allowed for selecting the optimal condition as 75% ethanol, 11 min and 20 °C. The optimal extracts showed high phenolic content (TPC = 350.80 ± 3.97 mg GAE/g extract) and antioxidant activity (ABTS, 9.31 ± 0.33 mmol Trolox/g extract), mainly composed of polymeric and mono-oligomeric flavan-3-ols. The digestion process reduced the TPC and antioxidant activity due to the low bioaccessibility of the flavan-3-ols, mainly as catechin, epicatechin and polymeric proanthocyanidin losses during the digestion process. However, increases in the antioxidant activity of the basolateral side (DDPH, 0.061 ± 0.000 mmol Trolox/g extract) were determined after in vitro transepithelial transport, which is a consequence of bioavailable catechin and epicatechin and reduced amounts of dimer B2, dimer B1, epicatechin gallate and gallic acid. Consequently, PLE combined with hydroalcoholic solvents at a low temperature resulted in a valuable methodology to obtain sustainable extracts from grape seed by-products (contributing to the circular economy), containing bioavailable phenolic compounds, which are able to increase the antioxidant status.

Optimization of the Process of Extracting Polysaccharides from Agrocybe aegerita and In Vitro Antioxidant and Anti-Aging Tests

The extraction process of crude polysaccharides from Agrocybe aegerita was optimized, and the antioxidant and anti-aging effects of the crude polysaccharides were evaluated. The optimal extraction parameters for the polysaccharide were identified using the response surface methodology. The DPPH, hydroxy radical, and superoxide anion radical scavenging capacities were evaluated to determine the antioxidant properties of the AAPs. The effects of the AAPs on the lifespan, head-swing frequency, swallowing frequency, body-bending frequency, and stress resistance of Caenorhabditis elegans were determined. The optimal extraction conditions included a solid-to-liquid ratio that resulted in an extraction solution concentration of 0.034 g/mL, an extraction temperature of 92.64 °C, and an extraction time of 2.82 h. Under these conditions, the yield of the AAPs was 11.325% ± 0.996%. The IC50 of the AAPs for superoxide anion radical scavenging was 4.693 mg/mL. The AAPs reached their maximum activity at concentrations of about 2 mg/mL for DPPH and 5 mg/mL for the hydroxyl radical. The AAPs could prolong the lifespan and improve locomotion and the stress resistance of C. elegans. Our findings illustrate the potential of AAPs as an anti-aging and antioxidant agent, highlighting the use of this natural compound in the fields of food and pharmacology.

Removal of Impurities from Nickel and Cobalt in Mixed Hydroxide Precipitate with Solvent Extraction Using Di(2-Ethylhexyl) Phosphoric Acid

ABSTRACT This study investigates the removal of major impurities, namely Fe, Al, Zn, and Mn, in a solution produced by sulfuric acid leaching of mixed hydroxide precipitate from the Ni and Co via solvent extraction using di(2-ethylhexyl) phosphoric acid (D2EHPA). The results of extraction experiments showed that the extracted Ni, Co, Fe, Al, Zn, Mn, and Mg increased as the equilibrium pH, D2EHPA concentration, and O/A ratio increased. The optimum extraction condition was achieved at a pH of 3.5, a 20% (v/v) D2EHPA concentration, and an O/A ratio of 1, with a complete (>99.9%) extraction of Al, Fe, Zn, and 97.33% Mn with co-extracted Ni and Co of 22.32% and 29.13%, respectively, in a single extraction stage. Complete Mn removal can be achieved in two extraction stages. Co-extracted Ni and Co can be scrubbed out using a mild sulfuric acid solution at a pH of 1.2 with only less than 2% of the Al, Fe, Zn, and Mn co-scrubbed. McCabe-Thiele diagrams of the scrubbing processes were constructed, and the results showed that Ni and Co can be scrubbed out using a mild acidic solution at a pH of 1.2, O/A ratio of 1, and temperature of 40°C for 10 min of mixing. Zn and Mn can be stripped completely using 0.5 M sulfuric acid solution at an O/A of 1 and temperature of 40°C for 10 min of mixing, while Fe and Al remained unstripped. Fe and Al can subsequently be stripped via reductive stripping.

Optimization of White Tea Flavanol Extraction Process by the Ultrasonic‐Assisted Deep Eutectic Solvent Method and Determination of the Antioxidant and Antibacterial Activity

ABSTRACTFlavanols have a variety of health benefits and biological activities and become the hotspot of the food development and research. In this research, flavanols were extracted from white tea by ultrasonic‐assisted deep eutectic solvent (DES) method. High‐performance liquid chromatography was used to determine the content of flavanols. The influence of four factors on the flavanol extraction yield was analyzed by single factor experiments, including deep eutectic solvent mole ratio (the mole of hydrogen bond acceptors: the mole of hydrogen bond donors), solid–liquid ratio (white tea sample weight/g: the volume of DES/mL), extraction time and extraction temperature. On the basis of single factor experiments, the factors which had significant effects on the flavanol extraction yield were further optimized by the response surface test. The results showed that the optimized extraction conditions were as follows: the mole ratio of DES 1: 4 (choline chloride: 1,2‐propanediol), the solid–liquid ratio 1:30, the extraction temperature 56°C, the extraction time 53 min, and the ultrasonic power 341 W. Under the above parameters, the extraction yield of white tea flavanols was 9.63 mg/g. After purification with macroporous resin, antioxidation and antibacterial experiments were carried out. The results showed that the antioxidant and antibacterial effects of white tea flavanols were remarkable. The antibacterial effects performed best on Escherichia coli, followed by Bacillus subtilis and Staphylococcus aureus. The maximum diameter of the antibacterial zone on Escherichia coli was 0.95 ± 0.11 mm. The best radical scavenging rates of OH, ABTS+ and DPPH were 97.1%, 97.5%, and 88.4%, respectively, when the flavanol concentration was 9.5 mg/mL. The conclusions of this research can provide theoretical foundation for the further study of white tea flavanols.

Efficient Extraction and Analysis of Wheat Straw Lignin by Response Surface Methodology

To enhance the high-value utilization of straw waste and achieve efficient lignin extraction, wheat straw was selected as the feedstock for investigating the effects of reaction temperature, reaction time, solid–liquid ratio, and formic acid concentration on lignin yield using a formic acid/acetic acid solvent system. A single-factor experimental design was initially employed, followed by optimization using the response surface methodology. Additionally, a kinetic model was developed to describe lignin extraction kinetics in the formic acid/acetic acid system. The structural characteristics and thermal stability of the extracted lignin were analyzed via FTIR, UV spectroscopy, and TGA. The findings indicate that increasing reaction temperature, reaction time, solid–liquid ratio, and formic acid content all significantly enhanced lignin extraction yield from wheat straw, with the primary influencing factors being reaction temperature > solid–liquid ratio > reaction time > formic acid content. The optimal extraction conditions were identified at a reaction temperature of 90 °C, a reaction time of 3.5 h, a solid–liquid ratio of 1:16.5, and a formic acid content of 86.2 wt.%, yielding a lignin content of 79.83%. The analytical results demonstrated that the extracted lignin preserved the structural integrity of the original lignin and exhibited good thermal stability.

Ultrasonic-Assisted Extraction and Antioxidant Evaluation of Resveratrol from Peanut Sprouts

The orthogonal array design method was used to optimize ultrasonic-assisted extraction of resveratrol from peanut sprouts. The results showed that the highest extraction yield of resveratrol using ultrasonic-assisted extraction could be up to 1.1%. The optimal extraction conditions were liquid to solid ratio of 30:1 (mL/g) and ethanol concentration of 80% (v/v) as solvent for 40 min at the temperature of 70 °C. AB-8 macroporous adsorption resin was used to purify the crude extract and the resveratrol content increased to 47.5% after one treatment run. The optimal adsorption parameters were initial concentrations in the sample solution of 2 mg/mL, a pH of 5.0, a flow rate of 2 mL/min, and a temperature of 25 °C. The optimal desorption parameters were 60% ethanol and a flow rate of 1 mL/min. The chemical composition of the peanut sprout’s resveratrol sample was investigated via HPLC, and the predominant constituents were found to be protocatechuic acid, catechins, caffeic acid, epicatechuic acid, resveratrol, and rutin. The antioxidant activities of the resveratrol were measured via the following different analytical methods: reducing power, 2,2-diphenyl-1-picrylhdrazyl (DPPH), hydroxyl radical-scavenger activity, superoxide radical-scavenger activity, the β-carotene bleaching test, and the scavenging nitrite test. The results indicated that the resveratrol in peanut sprouts have significant antioxidant activities and can be used as a source of potential antioxidant. And peanut sprout’s resveratrol has the potential and valuable application to be used as a new type of resveratrol resource. The finding of this study can provide some theoretical reference for the comprehensive utilization of peanut resources in the development of antioxidant health foods.

Optimization of Ultrasonic Extraction, Functional Properties, and Antioxidant Activity of Naematelia aurantialba Polysaccharides

AbstractNaematelia aurantialba (N. aurantialba) is a fungus rich in polysaccharides with medicinal and edible properties. Polysaccharides are the main active components of N. aurantialba; however, their biological activities and functional properties have not been widely explored. In this study, the ultrasonic extraction process for N. aurantialba polysaccharides (NAP) is optimized, and the physicochemical, functional, and antioxidant activities of the homogeneous fraction (NAP) are investigated. The optimal extraction conditions are a liquid–solid ratio of 50 mL g−1, ultrasonic power of 430 W, ultrasonic time of 32 min, resulting in an extraction rate of N. aurantialba polysaccharides of 48.68% ± 0.83%. NAP has a molecular weight of 915 kDa. The monosaccharide composition of NAP is as follows: mannose (59.04% ± 0.12%), xylose (23.89% ± 0.03%), glucuronic acid (14.07% ± 0.24%), galacturonic acid (2.12% ± 0.02%), and glucose (0.76% ± 0.02%). NAP exhibites water and oil retention capacities of 14.62 ± 0.25 g g−1 and 23.73 ± 0.85 g g−1, respectively. Furthermore, NAP demonstrates favorable moisture absorption and retention properties. The results show that NAP has a significantly stronger antioxidant effect, as demonstrated by its concentration‐dependent scavenging of ABTS, DPPH, and hydroxyl radicals.

Revealing the Potential of Star Anise Essential Oil: Comparative Analysis and Optimization of Innovative Extraction Methods for Enhanced Yield, Aroma Characteristics, Chemical Composition, and Biological Activities

ABSTRACTStar anise has been used for a long time in improving human health and curing diseases, owing to its unlimited components with complex chemical structures and a wide range of bioactivities. This study is aimed to investigate the influence of extraction methods (steam distillation, ethanol Soxhlet extraction, supercritical carbon dioxide extraction, subcritical n‐butane extraction) on the yield, aroma properties, chemical composition, and bioactivity of star anise essential oils. Electronic nose detection revealed the essential oils from subcritical extraction exhibited the most intense aroma, while the essential oils from ethanol Soxhlet extraction had a more complex aroma profile. Fourier‐transform infrared analysis showed the presence of benzene rings, carbonyl groups, C=C, and aromatic ether bonds in the essential oils extracted through different methods. The major components were heterocyclic olefins, heterocyclic oxygenates, and aromatic oxygenates, as well as certain amounts of flavonoids and polyphenols. Correlation analysis revealed the relative contents of volatile trans‐anethole, wormwood, d‐limonene, cineole, and trans‐α‐citronelene were strongly associated with the antibacterial activity of the essential oils. Similarly, the contents of volatile components (d‐limonene, cineole) and non‐volatile components (total flavonoids and total polyphenols) were strongly correlated with the DPPH scavenging activity of the essential oils. These results confirm the effectiveness of the ethanol Soxhlet extraction method in retaining the bioactivity of the essential oils. Finally, with a Box–Behnken central composite design of response surface and single‐factor experiments, the optimal extraction conditions for the ethanol Soxhlet method were determined: ultrasonic frequency of 80 kHz, crushing particle size of 60 meshes, liquid–material ratio of 8:1 (mL:g), and ultrasonic time of 35 min. Under these conditions, the essential oil yield was 25.51% ± 0.21%. Overall, these findings highlight the significance of extraction methods in obtaining high‐quality star anise essential oils with desirable aroma properties and potent bioactivities.

Optimization of the Cold Water Extraction Method for High-Value Bioactive Compounds from Chamomile (Matricaria chamomilla L.) Flower Heads Through Chemometrics.

This study focused on optimizing a cold water extraction method to obtain bioactive compounds from chamomile (Matricaria chamomilla L.), addressing increasing consumer demand for natural products and nutraceuticals. A full-factorial design was employed to evaluate the effects of temperature, time, and chamomile amount on the polyphenolic profile of extracts. The samples were characterized by HPLC-DAD and UV-Vis coupled with chemometrics; the analysis showed that extraction time negatively affected extract quality, as did the interaction between time and temperature. In addition, a significant positive quadratic effect for temperature and a positive coefficient for chamomile amount was found. ASCA was used to assess the UV-Vis profile, offering an alternative untargeted method for understanding the variable effects. The optimal extraction conditions (25 °C, 32 min, and 2.5 g of chamomile) produced samples high in hydroxybenzoic and hydroxycinnamic acids and flavanol derivatives. Using A face-centered design, this study also monitored antioxidant activity via a DPPH scavenging assay, confirming that the optimal conditions yielded samples within the range of maximum antioxidant activity in the studied experimental domain.

Sustainable separation of molybdenum from mixed mineral acids generated as semiconductor industry waste streams using tributyl phosphate (TBP) by effects of hybrid machine learning models

This study explores the separation and optimization of molybdenum (Mo) from mixed mineral acids derived from semiconductor industry waste streams with tributyl phosphate (TBP) by implementing machine learning (ML) models. Considerable experimental tests were performed to evaluate the impact of various operational variables on the effectiveness of Mo extraction and stripping. The support vector regression (SVR) paired with harmony search algorithm (HSA), genetic algorithm (GA), and shuffled frog leaping algorithm (SFLA) were employed for enhancement in the separation process and structural optimization. The SVR-SFLA model yielded the most meticulous predictions, identifying optimal extraction conditions with a TBP concentration, mixing time, temperature, and O/A ratio of 50%, 30 min, 25 °C, and 1, respectively, achieving 77.8% efficiency. The derived results from the SVR-SFLA model, in tandem with the McCabe-Theil diagram, indicated a four-stage counter-current extraction process required to achieve a yield exceeding 99%. For the stripping process, the hybrid model indicated optimal conditions with 3 M NH4OH and an A/O ratio of 0.5 at 50 °C for 20 min, requiring two counter-current stages for nearly complete stripping. Feature importance analysis using a random forest algorithm (RFA) highlighted the NH4OH concentration and phase ratio as the most significant factors, contributing 40.3% and 29.1%, respectively, to the stripping from the loaded TBP phase. The final product, obtained after crystallization and thermal decomposition of the strip solutions, was characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS), revealing 99.74% purity for molybdenum trioxide.

OPTIMIZATION ULTRASOUND-ASSISTED EXTRACTION USING CHOLINE CHLORIDE-BASED NATURAL DEEP EUTECTIC SOLVENT TO INCREASE PHENOLIC COMPOUNDS AND ANTIOXIDANTS FROM RHODOMYRTUS TOMENTOSA LEAVES

Objective: The main purpose of this study is to give recommendations for the ideal extraction conditions for improving the extraction yield and antioxidant activity of R. tomentosa leaves. Methods: First, the extraction total phenolic yields of five choline chloride-based Natural Deep Eutectic Solvents (NADES) were evaluated. Then, Box Behnken designs of Response Surface Methodology (RSM) were conducted in order to optimize the extraction condition. The extraction variables investigated were extraction time, water content in NADES, and solid-to-liquid ratio. Meanwhile, total phenolic and 2,2′-azinbis (3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) free radicals scavenging activity were used as responses. Results: NADES with combination of choline chloride and propylene glycol with a molar ratio of 1:1 was found to be the best solvent for extracting phenolic compound. The total phenolic compound obtained was 29.6351 mg GAE/g dried leaves with ABTS scavenging activity about 96.84% under the optimum extraction condition (extraction time of 60 min, 25% water content in NADES, and solid-to-liquid ratio of 0.02 g/ml). Better results were shown compared to extracts with conventional solvents. Conclusion: In sum, the use of choline chloride-based NADES as extraction solvent under optimum condition was proven to be effective in increasing the extraction efficiency of phenolic compounds and antioxidant activity from R. tomentosa leaves.

Optimizing polyphenol extraction and UPLC-MS/MS analysis from red clover (Trifolium pratense L.) species using response surface methodology

Polyphenols were extracted from red clover (Trifolium pratense L.) plants following conventional extraction. The combined factors of ethanol concentration (60–80%), extraction time (15–45 min) and extraction temperature (40–80°C) were evaluated. Central composite design software was used to conduct Response Surface Methodology (RSM) modelling and optimize the polyphenol yield from the red clover. Total phenolic content, antioxidant activity and ultra-performance liquid chromatography mass-spectrometry (UPLC-MS/MS) analysis were used to quantify polyphenols. The RSM model identified ethanolic composition having greatest influence (p < 0.05) on the polyphenol yield with extraction yields increasing with percentage ethanol. The optimal extraction conditions were identified as 80% ethanol for 45 minutes at 40°C. When compared with an exhaustive polyphenol extraction method (70% ethanol for 21 h at room temperature), the optimal extraction resulted in a 25.6% increase in TPC yield. UPLC-MS/MS was performed to quantify the individual polyphenols present within the sample, in which biochanin A and formononetin were present in abundance. The outcomes of this modelling and optimization study demonstrate that polyphenols from red clover can be extracted efficiently with minimal environmental and energy cost and thus had the capability to serve as a source of valuable nutraceutical and pharmaceutical products.

Optimization of Polysaccharide Extraction from Polygonatum cyrtonema Hua by Freeze–Thaw Method Using Response Surface Methodology

Polygonatum cyrtonema polysaccharides have a variety of pharmacological effects. The commonly used extraction methods include traditional hot water extraction, alkaline extraction, enzymatic hydrolysis method, ultrasonic-assisted extraction, etc., but there are problems such as low yield, high temperature, high cost, strict extraction conditions, and insufficient environmental protection. In this study, crude polysaccharide extraction from the Polygonatum cyrtonema Hua was performed using the freeze–thaw method. Response surface methodology (RSM), based on a three-level, three-variable Box–Behnken design (BBD), was employed to obtain the best possible combination of water-to-raw material ratio (A: 30–50), freezing time (B: 2–10 h), and thawing temperature (C: 40–60 °C) for maximum polysaccharide extraction. Using the multiple regression analysis and analysis of variance (ANOVA), the experimental data were fitted to a second-order polynomial equation and were used to generate the mathematical model of optimization experiments. The optimum extraction conditions were as follows: a water-to-raw material ratio of 36.95:1, a freezing time of 4.8 h, and a thawing temperature of 55.99 °C. Under the optimal extraction conditions, the extraction rate of Polygonatum cyrtonema Hua polysaccharide (PCP) was 65.76 ± 0.32%, which is well in close agreement with the value predicted by the model, 65.92%. In addition, PCP has significant antioxidant activity. This result shows that the freeze–thaw method can improve the extraction efficiency, maintain the structural integrity of polysaccharides, simplify the extraction process, promote the dispersion of polysaccharides, and is suitable for large-scale industrial production.