Ultrasound-assisted Deep Eutectic Solvent Research Articles

Eco-Friendly and Efficient Extraction of Polysaccharides from Acanthopanax senticosus by Ultrasound-Assisted Deep Eutectic Solvent.

A green extraction method was developed using deep eutectic solvent extraction for the polysaccharide from Acanthopanax senticosus (A. senticosus). Among the eight types of DES prepared, the DES with a ratio of 1:4 L-malic acid to L-proline was found to be a suitable extraction solvent based on the extraction efficiency. The extraction parameters were optimized by Plackett-Burman and response surface methodology (RSM). The best extraction conditions were found for L-malic acid. Under the conditions of an L-malic acid/L-proline ratio of 1:4, ultrasonic power of 240 W, material-liquid ratio of 31.068 g/mL, water content of 32.364%, extraction time of 129.119 min, and extraction temperature of 60 °C, the extraction rate of A. senticosus polysaccharides was 35.452 ± 0.388 mg-g-1. This rate was higher than that of polysaccharides obtained by hot water extraction (13.652 ± 0.09 mg-g-1). The experimental results were best fitted by the quasi-secondary kinetic model when compared to two other kinetic models. Electron microscopic observations showed that DESs were more destructive to plant cells. The polysaccharide extracted from DESs had more monosaccharide components, a lower molecular weight, a higher antioxidant capacity, and superior anti-glycation activity compared to polysaccharides extracted from water (ASPS-PW). This study demonstrates the effectiveness of DESs in obtaining polysaccharides from A. senticosus.

A Sustainable Extraction Approach of Phytochemicals from Date (Phoenix dactylifera L.) Fruit Cultivars Using Ultrasound-Assisted Deep Eutectic Solvent: A Comprehensive Study on Bioactivity and Phenolic Variability.

The present study aimed to evaluate the efficacy of natural deep eutectic solvents (NADESs) on the extraction of phytochemicals from eight Algerian date fruit cultivars (Phoenix dactylifera L.). In this study, lactic acid/sucrose-based NADESs were used as an alternative to conventional chemical solvents using the ultrasound-assisted extraction (UAE) method. The obtained extracts were assessed for the determination of bioactive compound contents, phenolic composition, antioxidant activity, and enzyme inhibitory potential. The results showed a considerable variation in phytochemical compositions and related activities between cultivars, where the greatest contents of total phenolics (1288.7 mg GAE/100 g), total flavonoids (53.8 mg QE/100 g), proanthocyanidins (179.5 mg CE/g), and total triterpenoids (12.88 mg OAE/100 g) were detected in the fruits of the Ourous cultivar. The same cultivar displayed the highest antioxidant capacity against DPPH• free radical (595 mg AAE/100 g), ABTS•+ cation radical (839 mg TE/100 g), and ferric reducing antioxidant potential (704 mg AAE/100 g). All extracts manifested moderate antioxidant activities tested by phosphomolybdenum, NO•, and linoleic acid lipid peroxidation assays. These extracts also exhibited interesting levels of in vitro enzyme inhibition; the Ourous cultivar gave the best inhibitory activity against α-amylase and acetylcholinesterase with 45 and 37%, respectively. HPLC-DAD-MS detected a total of five compounds, with phenolic acids and flavonoids being the main phenolics identified in the extract. The phenolic composition exhibited significant variability among cultivars. Notably, the highest amounts were revealed in the Tazizaout cultivar, with the predominance of gallic acid. The results confirmed that the combination of UAE and NADESs provides a novel and important alternative to chemical solvents for sustainable and environmentally friendly extraction and can represent a good alternative in food and pharmaceutical industry applications.

Optimization of ultrasound-assisted deep eutectic solvent extraction of polyphenols from Rhamnus alaternus for their antioxidant activity

Optimization of ultrasound-assisted deep eutectic solvent extraction of polyphenols from Rhamnus alaternus for their antioxidant activity

Ultrasound-assisted deep eutectic solvent extraction of bioactive compounds from persimmon calyx.

This study aimed to investigate the ultrasound-assisted extraction of bioactive compounds from persimmon (Diospyros kaki) calyx by deep eutectic solvents (DES) with different molar ratios. For this reason, the prepared DES extracts' total phenolic-flavonoid compounds and antioxidant activities (1,1-diphenyl-2-picrilhydrazyl radical scavenging activity [DPPH•], Cupric Reducing Antioxidant Capacity (CUPRAC), and ferric reducing antioxidant power [FRAP]) were investigated as a result of the experimental design and optimization study conducted for this purpose. A sonication time of 20min was determined as the optimal condition. Under these conditions, a molar ratio of 1.9:1 (lactic acid:choline chloride) and a water ratio of 70% provided the highest phenolic/flavonoid compounds and antioxidative activity. Correlations among water ratio, molar ratio, and sonication time were determined using principal component analysis (PCA). In conditions where total flavonoid compound, FRAP, and DPPH• are high due to PCA, it can be concluded that the sonication time is at high level; on the contrary, the water and molar ratios are at low level. In conclusion, ultrasound-assisted extraction using DES proved effective in persimmon calyx. Therefore, it can be recommended to use these environmentally friendly green solvents as an alternative to organic solvents in preparing extracts in various fields. PRACTICAL APPLICATION: This study shows the effectiveness of the ultrasound-assisted green extraction method using persimmon calyx specified as waste. These findings are compelling in the food industry in terms of consumers being now aware of green technology and the discovery that calyx is a good source of bioactive compounds.

Value-added green biorefinery co-products from ultrasonically assisted DES-pretreated Chlorella biomass

This study pursued the goal of creating value-added co-products through an environmentally friendly biorefinery approach, employing ultrasonically assisted deep eutectic solvent (DES)-pretreated Chlorella biomass. The primary focus was on generating enriched biodiesel feedstock with exceptional fuel properties and developing hydroponic biofertilizer. The results demonstrated the effectiveness of a two-step process involving a 5-minute ultrasound-assisted DES pretreatment followed by ultrasound-assisted solvent extraction, which efficiently extracted lipids from Chlorella biomass, yielding biodiesel-quality lipids with good cetane number (59.42) and high heating value (40.11 MJ/kg). Notably, this two-step approach (78.04 mg-lipid/g-microalgal biomass) led to a significant 2.10-fold increase in lipid extraction compared to a one-step process (37.15 mg-lipid/g-microalgal biomass) that combined ultrasound-assisted DES pretreatment and solvent extraction. Importantly, the aqueous extract derived from lipid-extracted microalgal biomass residues (LMBRs) showed promise as a component in hydroponic biofertilizer production, supporting lettuce growth in hydroponic deep water culture system. Consequently, microalgae biorefinery co-products hold tremendous potential in enhancing the profitability and sustainability of interconnected sectors, encompassing renewable energy, agriculture, and the environment.

Sustainable conversion of cottonseed hulls to valuable proanthocyanidins through ultrasound-assisted deep eutectic solvent extraction

This study presents a novel approach for converting cottonseed hulls (CSHs) into valuable proanthocyanidins (PAs) through deep eutectic solvent (DES)-based ultrasound-assisted extraction (UAE-DES). Response surface methodology (RSM) was applied to optimize and model this process, resulting in maximum yields of 78.58 mg/g. The ideal PA extraction conditions were determined to be a liquid-to-material ratio of 36.25 mL/g, a water content of 33.21%, and an extraction period of 7.4 min. Molecular dynamic simulations (MDS) were performed to study the interactions between the solvent and target chemicals. Increased van der Waals forces and stronger interactions between DES and the target chemical catechin (CA) compared to those observed with methanol or water were observed. Furthermore, the optimized extract exhibited a higher PA content than can be obtained with conventional extraction methods and demonstrated antioxidant activity in vitro. The cottonseed hulls residues (CSRs) remaining after the extraction process can be used to produce activated carbon (ACCSR), which has some capacity to adsorb methylene blue (MB) contaminants. This study offers a reference for the fruitful transformation of waste biomass into high-value products.

Ultrasound-Assisted Deep Eutectic Solvent Extraction of Phenolic Compounds from Thinned Young Kiwifruits and Their Beneficial Effects.

Fruit thinning is a common practice employed to enhance the quality and yield of kiwifruits during the growing period, and about 30-50% of unripe kiwifruits will be thinned and discarded. In fact, these unripe kiwifruits are rich in nutrients and bioactive compounds. Nevertheless, the applications of thinned young kiwifruits and related bioactive compounds in the food and functional food industry are still limited. Therefore, to promote the potential applications of thinned young kiwifruits as value-added health products, the extraction, characterization, and evaluation of beneficial effects of phenolic compounds from thinned young fruits of red-fleshed Actinidia chinensis cv 'HY' were examined in the present study. A green and efficient ultrasound-assisted deep eutectic solvent extraction (UADE) method for extracting phenolic compounds from thinned young kiwifruits was established. A maximum yield (105.37 ± 1.2 mg GAE/g DW) of total phenolics extracted from thinned young kiwifruits by UADE was obtained, which was significantly higher than those of conventional organic solvent extraction (CSE, about 14.51 ± 0.26 mg GAE/g DW) and ultrasound-assisted ethanol extraction (UAEE, about 43.85 ± 1.17 mg GAE/g DW). In addition, 29 compounds, e.g., gallic acid, chlorogenic acid, neochlorogenic acid, catechin, epicatechin, procyanidin B1, procyanidin B2, quercetin-3-rhamnoside, and quercetin-3-O-glucoside, were identified in the kiwifruit extract by UPLC-MS/MS. Furthermore, the contents of major phenolic compounds in different kiwifruit extracts prepared by conventional organic solvent extraction (EE), ultrasound-assisted ethanol extraction (UEE), and ultrasound-assisted deep eutectic solvent extraction (UDE) were compared by HPLC analysis. Results revealed that the content of major phenolics in UDE (about 15.067 mg/g DW) was significantly higher than that in EE (about 2.218 mg/g DW) and UEE (about 6.122 mg/g DW), suggesting that the UADE method was more efficient for extracting polyphenolics from thinned young kiwifruits. In addition, compared with EE and UEE, UDE exhibited much higher antioxidant and anti-inflammatory effects as well as inhibitory effects against α-glucosidase and pancreatic lipase, which were closely associated with its higher content of phenolic compounds. Collectively, the findings suggest that the UADE method can be applied as an efficient technique for the preparation of bioactive polyphenolics from thinned young kiwifruits, and the thinned young fruits of red-fleshed A. chinensis cv 'HY' have good potential to be developed and utilized as functional foods and nutraceuticals.

Total biflavonoids extraction from Selaginella chaetoloma utilizing ultrasound-assisted deep eutectic solvent: Optimization of conditions, extraction mechanism, and biological activity in vitro

In this study, the deep eutectic solvent based ultrasound-assisted extraction (DES-UAE) was investigated for the efficient and environmentally friendly extraction of Selaginella chaetoloma total biflavonoids (SCTB). As an extractant for optimization, tetrapropylaminium bromide-1,4-butanediol (Tpr-But) was employed for the first time. 36 DESs were created, with Tpr-But producing the most effective results. Based on response surface methodology (RSM), the greatest extraction rate of SCTB was determined to be 21.68 ± 0.78 mg/g, the molar ratio of HBD to HBA was 3.70:1, the extraction temperature was 57 °C, and the water content of DES was 22 %. In accordance with Fick's second rule, a kinetic model for the extraction of SCTB by DES-UAE has been derived. With correlation coefficients 0.91, the kinetic model of the extraction process was significantly correlated with the general and exponential equations of kinetics, and some important kinetic parameters such as rate constants, energy of activation and raffinate rate were determined. In addition, molecular dynamics simulations were used to study the extraction mechanisms generated by different solvents. Comparing the effect of several extraction methods on S.chaetoloma using ultrasound-assisted extraction and conventional methods, together with SEM examination, revealed that DES-UAE not only saved time but also enhanced SCTB extraction rate by 1.5–3 folds. SCTB demonstrated superior antioxidant activity in three studies in vitro. Furthermore, the extract could suppress the growth of A549, HCT-116, HepG2, and HT-29 cancer cells. Alpha-Glucosidase (AG) inhibition experiment and molecular docking studies suggested that SCTB exhibited strong inhibitory activity against AG and potential hypoglycemic effects. The results of this study indicated that a Tpr-But-based UAE method was suitable for the efficient and environmentally friendly extraction of SCTB, and also shed light on the mechanisms responsible for the increased extraction efficiency, which could aid in the application of S.chaetoloma and provide insight into the extraction mechanism of DES.

Dietary Fiber from Navel Orange Peel Prepared by Enzymatic and Ultrasound-Assisted Deep Eutectic Solvents: Physicochemical and Prebiotic Properties.

Dietary fiber (DF) was extracted from navel orange peel residue by enzyme (E-DF) and ultrasound-assisted deep eutectic solvent (US-DES-DF), and its physicochemical and prebiotic properties were characterized. Based on Fourier-transform infrared spectroscopy, all DF samples exhibited typical polysaccharide absorption spectra, indicating that DES could separate lignin while leaving the chemical structure of DF unchanged, yielding significantly higher extraction yields (76.69 ± 1.68%) compared to enzymatic methods (67.27 ± 0.13%). Moreover, ultrasound-assisted DES extraction improved the properties of navel orange DFs by significantly increasing the contents of soluble dietary fiber and total dietary fiber (3.29 ± 1.33% and 10.13 ± 0.78%, respectively), as well as a notable improvement in the values of water-holding capacity, oil-holding capacity, and water swelling capacity. US-DES-DF outperformed commercial citrus fiber in stimulating the proliferation of probiotic Bifidobacteria strains in vitro. Overall, ultrasound-assisted DES extraction exhibited potential as an industrial extraction method, and US-DES-DF could serve as a valuable functional food ingredient. These results provide a new perspective on the prebiotic properties of dietary fibers and the preparation process of prebiotics.

Optimization of ultrasound-assisted deep eutectic solvent extraction of bioactive compounds from pomegranate peel using response surface methodology.

The efficient extraction of polyphenols from pomegranate peels using a deep eutectic solvent (DES) and ultrasound-assisted extraction (UAE) was investigated. A Box-Behnken design was used to investigate the effects of four independent variables (water content, liquid-to-solid ratio, ultrasonic power, and extraction time) on total polyphenol content (TPC), punicalagin content (PC), and ellagic acid content (EC). Optimized DES-based UAE conditions were as follows: TPC (water content, 29.30%; liquid-to-solid ratio, 53.50 mL/g; ultrasonic power, 238.20W; extraction time, 29.50min), PC (water content, 25.65%; liquid-to-solid ratio, 44.20 mL/g; ultrasonic power, 120W; extraction time, 20min), and EC (water content, 33.13%; liquid-to-solid ratio, 60 mL/g; ultrasonic power, 300W; extraction time, 20min). Under these optimal conditions, the experimental values for TPC, PC, and EC were 67.50mg GAE/g, 130.65mg/g, and 2.04mg/g, respectively; these values were consistent with the predicted values.

Ultrasonic assisted extraction of anthocyanins from rose flower petal in DES system and enzymatic acylation

Herein, the anthocyanins from rose were extracted, purified and identified by ultrasound-assisted deep eutectic solvents (DES), the resin, and ESI-Q-TOF-MS, respectively. The purified anthocyanins were modified through acylation by means of enzymatic catalysis method to improve the stability of anthocyanins. Compared with traditional extraction agents (ethanol), anthocyanins extraction rate was significantly improved when choline chloride/lactic acid was chosen as extraction solvent, and reached 8.265 mg g−1. The ESI-Q-TOF-MS detection results showed that the main component of the anthocyanins was peonidin-3,5-di-O-glucoside with 65.93% content. Meanwhile, the maximal acylation rate was 95.13% under optimal conditions (0.25 g of anthocyanin, 2.5 mL of pyridine, 4 mL of methyl benzoate; 400 mg of Novocain 435 lipase addition; a water bath at 50 °C under negative pressure of 0.09 Mpa for 9 h). Furthermore, the loss rate of acylated anthocyanins was significantly lower than that of natural anthocyanins under the same temperature or light conditions, and the acylation of anthocyanin could significantly improve stability against temperature, light and pH. The acylated anthocyanin exhibited excellent free radical scavenging activities for DPPH and ABTS+, and IC50 values (4.451 μg mL−1 for DPPH and 7.760 μg mL−1 for ABTS+) displayed its high antioxidant activity.

Ultrasound and deep eutectic solvent as green extraction technology for recovery of phenolic compounds from Dendrobium officinale leaves

Ultrasound and deep eutectic solvent (DES) are two green and efficient techniques in extraction. In this study, an eco-friendly extraction of phenolic compounds from Dendrobium officinale leaves (DOLs) was investigated. Ten DESs containing choline chloride, betaine, organic acids, polyols and amide, were tailored for extraction. Choline chloride-oxalic acid showed the most promising efficiencies for phenolics as 9.84 ± 0.19 mg GAE/g DW. Ultrasound-assisted DES (UADES) were optimized by a Box-Behnken design of response surface methodology. The optimum conditions were ultrasonic power 330 W, extraction temperature 60 ℃, and liquid-solid ratio 53:1 mL/g with a total phenolic content (TPC) of 17.50 ± 0.35 mg GAE/g DW. Compared with a single or triple frequency ultrasound, a dual-frequency of 40/60 kHz treatment for 15 min made TPC up to be 25.15 ± 1.46 mg GAE/g DW. About 13 phenolics were identified by UPLC-Triple-TOF/MS as the crucial phenolics in extracts, such as rutin and apigenin flavonoids. In addition, leave surface changed dramatically by UADES. These phenolic extracts had eminent antioxidant capacities, such as DPPH• scavenging rate of 65.4% and FRAP value of 0.234 mmol/L FeSO4 at TPC of 4 mg/mL. Accordingly, dual-frequency UADES is a meaningful and green technology for extraction of phenolic compounds.

Sequential ultrasound assisted deep eutectic solvent-based protein extraction from Sacha inchi meal biomass: towards circular bioeconomy.

The need for high-quality dietary proteins has risen over the years with improvements in the quality of life. Deep eutectic solvents (DESs) have been regarded as potential green alternatives to conventional organic solvents for protein extraction from press cake biomass, meeting the needs of sustainable development goals. Sacha inchi seed meal (SIM) is generated as a by-product of the seed oil extraction industries containing high protein content. The current study presents a novel ultrasound assisted DES method for the extraction of SIM protein in a sequential manner. Four different DESs were screened, out of which choline chloride (ChCl)/glycerol (1:2) gave promising results in protein recovery and was further selected. The sequential ultrasound-ChCl/glycerol could effectively extract high total crude protein content (77.43%) from SIM biomass compared to alone ultrasound (29.21%) or ChCl/glycerol (58.32%) treatment strategies. The SIM protein extracted from ultrasound-ChCl/glycerol exhibited high solubility (94.39%) at alkaline pH and highest in vitro digestibility (71.16%) by digestive enzymes (pepsin and trypsin). The protein characterization by SDS-PAGE and FTIR elucidated the structural properties and presence of different functional groups of SIM protein. Overall, the sequential ultrasound-ChCl/glycerol revealed its significant potential for one-step biorefining of the waste Sacha inchi meal biomass for circular bioeconomy.

Ultrasound-Assisted Deep Eutectic Solvent Extraction of Polysaccharides from Anji White Tea: Characterization and Comparison with the Conventional Method.

Deep eutectic solvent as a new green and safe solvent system has attracted more and more attention in recent years. In this study, three deep eutectic solvents (DES) were combined with ultrasound irradiation to extract tea polysaccharides (TPs) from Anji white tea, which was compared with conventional hot water extraction (HW). The physicochemical, structural, and biological properties of TPs extracted by ultrasound-assisted DES and hot water (HWP) were further investigated. Results showed that the DES system composed of choline chloride and 1,6-hexanediol (CH) with the molar ratio of 1:2 exhibited the optimal extraction yield (19.18%) and in vitro antioxidant activities for TPs (CHP). Furthermore, compared to the HWP, the CHP had a higher extraction yield and total carbohydrate content and a lower molecular weight. Monosaccharide composition analysis displayed that the molecular structure of CHP exhibited more arabinose but less glucose, mannose, galacturonic acid, and glucuronic acid than HWP. Little difference was observed in the preliminary structural characteristics between HWP and CHP from Fourier transform infrared analysis. Besides, CHP possessed better α-glucosidase inhibitory and hypoglycemic activity in L6 cells than HWP. Therefore, the ultrasound-assisted DES extraction method can be a promising strategy for extracting TPs with excellent bioactivities for future applications in functional foods.

Optimization of ultrasound-assisted deep eutectic solvent extraction of betanin and its application in chitosan-based biofilm

Optimization of ultrasound-assisted deep eutectic solvent extraction of betanin and its application in chitosan-based biofilm

An environment-friendly approach using deep eutectic solvent combined with liquid-liquid microextraction based on solidification of floating organic droplets for simultaneous determination of preservatives in beverages.

With the increase in environmental protection awareness, the development of strategies to reduce the use of organic solvent used during the extraction process has attracted wide attention. A simple and green ultrasound-assisted deep eutectic solvent extraction combined with liquid-liquid microextraction based on solidification of floating organic droplets method was developed and validated for the simultaneous determination of five preservatives (methyl paraben, ethyl paraben, propyl paraben, isopropyl paraben, isobutyl paraben) in beverages. Extraction conditions including the volume of DES, value of pH, and concentration of salt were statistically optimized through response surface methodology using a Box-Behnken design. Complex Green Analytical Procedure Index (ComplexGAPI) was successfully used to estimate the greenness of the developed method and compare with the previous methods. As a result, the established method was linear, precise, and accurate over the range of 0.5-20 μg mL-1. Limits of detection and limits of quantification were in the range of 0.15-0.20 μg mL-1 and 0.40-0.45 μg mL-1, respectively. The recoveries of all five preservatives ranged from 85.96% to 110.25%, with relative standard deviation less than 6.88% (intra-day) and 4.93% (inter-day). The greenness of the present method is significantly better compared with the previous reported methods. Additionally, the proposed method was successfully applied to analysis of preservatives in beverages and is a potentially promising technique for drink matrices.

A novel strategy to improve the recovery of phenolic compounds from Pistacia lentiscus L. fruits using design-based statistical modeling for ultrasound-deep eutectic solvents extraction and the evaluation of their antioxidant potential

Recently, there has been increasing interest in using alternative green technologies for the isolation of bioactive metabolites from medicinal plants. This study was designed to select the optimal solvent for phenolic compounds (TPC) extraction from Pistacia lentiscus L. black fruits (PBF) and the development of an experimental model by response surface methodology using ultrasound-assisted deep eutectic solvents (UAE-DES). The characterization and the antioxidant capacity of PBF phytochemicals using a multi-test system in-vitro were investigated. The highest amount of phenolic compounds (TPC: 183.95 ± 0.01 mg GAE/Gdw) was obtained using choline chloride-acetic acid solvent DES, under the optimum extraction conditions: 28.3% of water percentage, 40 °C of extraction temperature, and 18 min of extraction time. Moreover, DES extract had a more important antioxidant capacity with no significant difference compared to the control (Ascorbic acid). Furthermore, HPLC-DAD and TLC analysis indicated the presence of rutin and Cyanidin-3-glycoside in fraction number 4 after fractionation using the HP-20 diaion resin column. This extraction media has proved to be an alternative approach for the extraction of bioactive compounds as a sustainable and safe extraction media for pharmaceutical and industrial applications.

Biomass valorization by integrating ultrasonication and deep eutectic solvents: Delignification, cellulose digestibility and solvent reuse

Biomass valorization in converting biomass into value-added products and energy has gained researchers’ attention. In this study, valorization of oil palm empty fruit bunch (OPEFB) towards biofuels production was focused. Combination of deep eutectic solvent (DES) and ultrasonication was employed to pretreat the OPEFB. The pretreatment was conducted in a sonicator at 210 W, 50 °C for 30 min. Choline chloride-lactic acid (ChCl-LA) outperformed choline chloride-urea (ChCl-U) and choline chloride-glycerol (ChCl-G) because of its acidity and low viscosity properties. Besides having the highest cellulose digestibility (36.7% of reducing sugars yield), ChCl-LA pretreated biomass had the lowest lignin content of 18.8% and biomass crystallinity of 0.895. Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) results further confirmed its biomass disruption ability. Ultrasonic-assisted DES pretreatment exhibited a synergetic effect, whereby the reducing sugars yield was double compared to without ultrasound. Also, its pretreatment performance was better than other pretreatment methods, such as acid, alkaline and steam explosion pretreatments. The DESs were effectively recovered with a slight decrease in delignification and cellulose digestibility efficiencies. These collectively proven the feasibility and effectiveness of ultrasound-assisted DES pretreatment in converting the biomass to sugars, which could be essential for biofuels production.

Extraction and recovery of chlorogenic acid from sunflower disks using a high‐efficiency system composed of deep eutectic solvents and macroporous resins

Conventional methods to extract and recover chlorogenic acid (CGA) from plants exhibit plenty of flaws, like over-consumption of organic solvents, low extracting rate, and low enrichment efficiency. Herein, an ultrasound-assisted deep eutectic solvent extraction (UAE-DESs) was introduced to extract CGA from sunflower disks. And NKA-II macroporous resin was used as adsorbent to adsorb CGA from dilute DESs extracts. Then NKA-II was collected by filtration followed by desorption to obtain CGA separated from DESs. The extraction yield of CGA was 6.16 mg/g with liquid–solid ratio 31 ml/g, ultrasonic temperature 47°C, ultrasonic time 54 min, and deep eutectic solvent (DES) composed of choline chloride/1,4-butanediol (1/2, mol/mol) and water content 30% (w/w). After NKA-II enrichment, the recovery efficiency of CGA was 80.76% and the purity was 75.84%. Moreover, the recovered DESs could be reused during the extraction. The present research provided a time-saving, green, and sustainable method for extracting and recovering CGA from sunflower disks. Practical applications The research proposed a method for the extraction and recovery of CGA from sunflower disks by combining UAE-DESs and NKA-II macroporous resins. The combination of diluted DESs with macroporous resins can effectively overcome the disadvantages of DESs and provide an efficient method for the recovery of natural products. The CGA extracted can be applied in medicine, food, and other fields.

Iridoid Glycosides from Phlomis Medicinalis Diels: Optimized Extraction and Hemostasis Evaluation.

Phlomis medicinalis Diels, an important perennial herbal plant unique to the Qinghai-Tibet Plateau, is often used as Tibetan Materia Medicine Radix Phlomii for the treatment of cold, cough, and convergence trauma. In order to efficiently extract the iridoid glycosides from P. medicinalis, an ultrasound-assisted deep eutectic solvent extraction technique was employed. The main parameters influencing the extraction process were studied through single-factor tests and the extraction was optimized by using response surface methodology. The hemostasis activity of total iridoid glycosides (TIG) from P. medicinalis was evaluated in vitro and in mice. The optimization results revealed that the optimal process parameters were liquid-solid ratio 20 : 1, choline chloride-lactic acid concentration 79 %, and sonication time 34 min, under which a TIG extraction yield of 20.73 % was obtained. Meanwhile, high-performance liquid chromatography-photodiode array/mass spectrometry (HPLC-PDA/MS) was employed to characterize the optimized extract and indicated that TIG from P. medicinalis mainly consisted of sixteen reported iridoid glycosides with a total content of 91.22 %. The experimental results in vivo and in vitro indicated that TIG from P. medicinalis had strong hemostasis activities, which may be achieved by increasing the fibrinogen levels. Therefore, the ultrasound-assisted deep eutectic solvent extraction is an effective method to extract iridoid glycosides from P. medicinalis and they will be promising candidates to be developed for medical hemostasis agents.