Solvent Ratio Research Articles

Obtaining the Enoxaparin Sodium Substance Equivalent to the Original Clexane® and Lovenox®. The Selection of Technological Parameters and Optimization of the “Greenness” of the Purification Stage

The aim of the study was to adjust and optimize the purification stage of crude enoxaparin sodium to obtain a substance equivalent to the original drugs Clexane® and Lovenox® according to the criteria specified by the FDA. The purification stage involves the reprecipitation of crude enoxaparin in methanol. Determining the ratio of solvents required for the reprecipitation is important for studying the correlation between the experimental conditions of the technological process and the structural characteristics of enoxaparin samples. In the study, the method of purification of enoxaparin sodium described in the patent was assessed, and the following variations of the MeOH:H2O solvent ratio were selected – 4:1; 2:1; 1:1. The obtained samples of enoxaparin sodium were analyzed according to the in-house specification developed on the basis of the pharmacopoeial monograph, as well as by non-pharmacopoeial methods, such as two-dimensional NMR spectroscopy (HSQC) and size exclusion chromatography (SEC) for detailed characterization of the molecule. Strategies of greening of the enoxaparin sodium purification stage by reducing the E-factor were also considered in the study. Considering the principles of “green” chemistry, the method of purification of crude enoxaparin sodium was optimized by the solvent regeneration. It was experimentally possible to demonstrate the effect of the solvent ratio at the stage of purification of crude enoxaparin on the composition, as well as on the number and distribution of oligosaccharide fractions in the molecule. Based on the results of the study, it can be concluded that the ratio of MeOH:H2O=1:1 allows obtaining samples that are closest to Clexane® and Lovenox® in terms of the molecular weight distribution profile and the composition profile. The E-factor was also reduced from 14 to 5.25 by solvent regeneration.

Kinetics of Essential Oil Extraction of Kaffir Lime Peel Using Microwave Assisted Hydrodistillation

The purpose of this study is to study the kinetics of kaffir lime peel essential oil extraction using microwave assisted hydrodistillation. Extraction was carried out at various powers and the ratios of material to solvent for 1 hour. Soxhlet extraction using n-hexane solvent was also carried out to determine the yield of essential oil. The extraction kinetics was investigated using a mass transfer-controlled approach and expressed by the 1st and 2nd order of reaction rate. The Soxhlet extraction results indicated that the yield of kaffir lime peel essential oil was 5.65% w/w. The higher the microwave power being applied (180, 300, 450, and 600 Watt), the higher the essential oil yielded (2.2; 2.8; 3; and 3.8% w/w), respectively, but at 800 Watt, the yield decreased (3.2% w/w). The smaller the ratio of material to solvent, which means more diluted, the lower the yield of oil were, namely from 4.56; 3.9; and 3.8% w/w, at ratios of material to solvent 1:3, 1:3.5, and 1:4 w/v. Different results were obtained at a ratio of 1:3 (4.56% w/w) which produced a yield greater than the ratio of 1:1.25 (2.88% w/w). Therefore, the optimum conditions for extracting kaffir lime peel essential oil were at 600 Watt and a ratio of material to solvent 1:3 w/w for 56 minutes with a yield of 4.58% and a density of 0.86 g/cm3. The kinetics of the 2nd order of homogeneous model better represented results of the experiments with extraction rate constants at 180, 300, 450, 600, and 800 Watt of 14.89; 14.95; 15.53; 21.32; and 19.85 L.g-1.min-1. While the extraction rate constants at the material to solvent ratio of 1:2.5; 1:3; 1:3.5; and 1:4 w/v of 17.38; 19.80; 22.09; and 32.31 L.g-1.min-1. The extraction capacity was also affected by the power and the ratio of material to solvent, the extraction capacity were 0.0095; 0.0100; 0.0104; 0.0125; and 0.0106 g.L-1, at 180, 300, 450, 600, and 800 Watt respectively, and 0.0094; 0.0134; 0.0134; and 0.0118 g.L-1, at material to solvent ratio of 1:2.5; 1:3; 1:3,5; and 1:4 w/v respectively.

Kinetic modeling of phenolic compounds extraction from nutshells: influence of particle size, temperature and solvent ratio

This paper studies the effects of particle size, temperature and ethanol–water solvent ratio on the extraction of total phenolic compounds (TPC) from peanut, coconut, and macadamia nutshells. Using an I-optimal design, the maximum TPC extraction obtained from the shells ranged from 63.5 ± 1.6 to 76.2 ± 3.1 mg gallic acid equivalent (GAE) per 100 g dry weight (dw) of nutshell. Next, a response surface model (RSM) was developed to describe the relationship between the process parameters and the extracted TPC concentration, in order to predict the optimal extraction conditions. For all of the examined biomasses, the optimal conditions for extraction were predicted at a particle size of 1 mm, temperature of 75 °C and ethanol/water mixture of 54, 53 and 65% ethanol, for peanut, coconut and macadamia nutshells respectively. Particle size seems to be the most important parameter, while temperature appears to be of lesser importance. Besides, the extraction kinetics were assessed by fitting kinetic models on the experimental data. The combined second-order diffusional model provided the best goodness of fit. This model revealed that, at the boundary layer, the effect of washing mechanism of extraction is more important than extraction due to diffusion kinetics. This study provides an understanding of the mass transfer mechanism involved in the TPC extraction process from nutshells, which yields valuable insights that could facilitate the industrial biorefinery of nutshells.Graphical

Flower-shaped covalent organic framework synthesis and its anticancer drug delivery application

Fabrication of covalent organic frameworks (COFs) at room temperature is necessary due to their easy preparation, practical scale-up, and low cost to overcome the limitations of solvothermal and high-temperature synthesis. Herein, we fabricated flower-shaped COFs (FSCOFs) that were synthesized in various ratios of ortho-xylene and butanol mixture solvents. The FSCOFs exhibited excellent crystallinity with a pore size of approximately 10 nm, which was confirmed by PXRD and BET measurements. To utilize the FSCOFs as a drug carrier, doxorubicin (DOX) was loaded, followed by encapsulation of hyaluronic acid to increase the colloidal stability of FSCOFs in a physiological environment (FSCOFs-DOX-HA). The encapsulation efficiency and the drug loading capacity of FSCOFs-DOX-HA were 21.23 % and 29.82 %, respectively. Moreover, 92 % and 59 % of DOX is released in acidic environments and elevated GSH environments, proving the sensitivity of the FSCOFs as carriers. The excellent drug release mechanism of FSCOFs-HA-DOX is demonstrated by FSCOFs imine nitrogen protonation under acidic environment confirmed by its zeta potential changes under various physiological environments. The designed FSCOFs-DOX-HA was demonstrated to be a pH-sensitive drug carrier to deliver anticancer drugs into cancer cells. The MTT and drug internalization data demonstrated sustained DOX release from FSCOFs-DOX-HA. Finally, the real-time fluorescence demonstrates the effectiveness of the FSCOFs-DOX-HA upon cellular uptake and release of the anticancer drug. Thus, the FSCOFs system reported here opens a new path in COF research for drug carrier systems.

Transparency and Thermal Stability of Silica Aerogel Synthesized From Sodium Silicate Using Ambient Pressure Drying

Silica aerogel is a special material due to its low density, high transparency, and high thermal stability. Producing silica aerogels in an inexpensive and environmentally friendly way is the focus of recent research. Here, silica aerogel is synthesized from sodium silicate as silica source and surface modification with organosilanes, followed by ambient pressure drying at various conditions. The resulting aerogels were analyzed for their density, transparency, and thermal stability. Silica aerogel with a low density of 0.4031 g/cm3 was successfully synthesized with polydimethylsiloxane (PDMS) as modifying agent at 7:50 solvent ratio. The aerogel can withstand heat up to 400°C.This shows the potential of aerogel to be applied as thermal insulator in various fields.

Drying method comparison of black mangrove leaves (Rhizophora mucronata) for an antioxidant activity assay

Ethanolic extracts of black mangrove leaf (Rhizophora mucronata) can be a natural source of antioxidants. The phenolic content can affect the activity of antioxidants in the sample. This study aimed to determine black mangrove leaf (Rhizophora mucronata) chemical content primarily focused on total phenolic content and antioxidant activity during sun and wind drying using DPPH, ABTS and CUPRAC analysis methods. Ethanolic extracts were obtained from the maceration method with 1:5 sample and solvent ratio. The total phenolic content value was 1691.2 mg GAE/g with an extract yield of 12.57%. The antioxidant activity of DPPH, ABTS, and CUPRAC method values were 16.61 ppm, 11.07 ppm and 103.52 mg ascorbic acid/g extract and classified as a very strong antioxidant. The best result showed that the highest content of phenolic content and antioxidant activity could be found in the wind-dried extract. The result indicated that ethanolic extract of Rhizophora mucronata leaves can be utilized as a strong antioxidant agent. Drying methods can be used as a good way to preserve mangrove leaves while maintaining their antioxidant activity.

Extraction Study of Black Pepper (Piper nigrum l.) Using Ultrasound-Assisted Extraction Method

Piper nigrum l. or black pepper, is a plant native to Indonesia that grows in Malaysia, Sri Lanka, Vietnam, and other Southeast Asian countries. Black pepper is processed into oleoresin by extraction. Ultrasound-assisted extraction is a method to increase the yield and efficiency of oleoresin extraction. This study aimed to examine the effect of extraction time and temperature on yield, density, refractive index, study chemical components of black pepper oleoresin, and assess the best relative results according to SNI 01-0025-1987-B. Black pepper powder was extracted by ultrasound using ethanol solvent. The ratio of material and solvent used is 0.37 w/v. The operating conditions were carried out at extraction times of 20, 35, 50, 65, and 80 minutes and extraction temperatures of 30, 40, 50, 60, and 70 ˚C with a frequency of 40 kHz. The results showed that increasing the extraction time and temperature caused the yield, density, and refractive index values to be greater. The best relative results at 80 minutes and 70˚C with a dark brown color, in the form of a liquid paste, with a distinctive pepper aroma, yield 22.57%, density 0.8350 gram/ml, piperine content 74.78%, content 25.22 %, and a refractive index of 1.4900

Pengaruh Variasi dan Konsentrasi Pelarut Terhadap Yield Antosianin Ekstrak Bunga Telang (Clitoria ternatea L.) Sebagai Pewarna Alami

One of these resources that may be used as a source of natural dyes is the telang flower (Clitoria ternatea L). Telang flower contains anthocyanin pigments that give it a blue color so that it can be used as a natural dye that can be applied to food or drinks. The purpose of this study was to determine the anthocyanin levels in the telang flower extract using various types of solvents and solvent concentrations. The solvent variations used were acetic acid, citric acid, and tartaric acid with solvent concentrations of 0.5, 1, 1.5, and 2% (w/v). The method used in this research is the maceration extraction method with a maceration time of 25, 50, 75, and 100 minutes. The results obtained The type of acid, namely acetic acid, citric acid, and acetic acid affected the anthocyanin yield, with values of 0.4729, 0.758, and 0.785 respectively at a solvent ratio of 1: 6. Variation of solvent concentration from 0.5%, 1 %, 1.5%, and 2% (v) 2% (v) acetic acid solvent can produce a maximum anthocyanin yield of 0.254 g/5 g, citric acid is 0.317 mg/5 gram, and tartaric acid is 0.343 at a concentration of 2% ( b/v).

Extraction of Flavonoid Content from Banana Peel (Musa Paradisiaca L.) by Ultrasound – Assisted Extraction Method and Its SPF Value

In this study, banana peel was used as a natural sunscreen compound because of its natural antioxidants, such as flavonoids, tannins, triterpenoids, and phenols. Extraction is carried out using Ultrasound-Assisted Extraction method with variations in ethanol solvent concentration and material to solvent ratio at 45oC for 45 minutes. The ethanol concentrations used are 96%, 70%, and 50% and the material to solvent ratio 1/10, 1/20, and 1/30. From the results of the study, the highest yield and SPF value were obtained at ethanol concentration of 50% and material to solvent ratio 1/30. The yield in this variation is 15.2646%, and the SPF value is 8.9874 with the maximum protection category. The highest Total Flavonoid Content (TFC) results was obtained at 70% ethanol concentration and the ratio of material to solvent 1/30, namely 1.6559 mg QE/g. From the variation with the best TFC value, the mass transfer coefficient is 0.0151 mL/µg QE.min.

Total Triterpenes, Polyphenols, Flavonoids, and Antioxidant Activity of Bioactive Phytochemicals of Centella asiatica by Different Extraction Techniques.

Obtaining phytochemical-rich plant extracts from natural products where the active ingredients are present in comparatively low levels in the tissue matrix is the critical initial step of any chemical analysis or bioactivity testing. The plant C. asiatica is rich in various phytochemicals, the major constituents being triterpenes and flavonoids, as well as other polyphenols, leading to a number of bioactivities. In this study, an attempt was made to achieve several green technology principles, while optimizing the extraction method for the efficient extraction of bioactive compounds from C. asiatica. Soxhlet extraction (SE), ultrasound-assisted extraction (UAE) with low-frequency sonication, microwave-assisted extraction (MAE) using a closed-vessel microwave digestion system, and subcritical water extraction (SWE) in a high-pressure reactor were employed to extract the bioactive compounds. The solvent system, extraction time, and solid-to-solvent ratio were varied to optimize the extraction. UAE gave the best extraction yield, while MAE gave similar results, with a solid-to-liquid ratio of 1:25, a binary solvent system of 9:1 methanol to water (v/v), and a 20 min extraction time for the extraction of triterpenes, including madecassoside, asiaticoside, madicassic acid, and asiatic acid. Investigation of different solvent systems based on water and methanol also revealed information on the extraction behavior of total triterpene content (TTC), total polyphenolic content (TPC), total flavonoid content (TFC), and the variations in the antioxidant capacity of the extracts. In this study, it was evident that UAE and MAE offer more efficient and effective extraction of bioactive compounds in terms of extraction yield, time, and minimal solvent and energy use. Furthermore, the results showed that the different solvent ratios in the extraction mixture will affect the extraction of bioactive compounds, and a binary solvent system with a combination of methanol and water was the most efficient for the studied compounds in Centella asiatica.

Effect of Stirring Speed and Solid to Solvent Ratio on Fucoidan Yield from Sargassum sp.

Effect of Stirring Speed and Solid to Solvent Ratio on Fucoidan Yield from Sargassum sp.

Simulation of Furfural and Levulinic Acid Production from Lignocellulosic Biomass

Furfural and levulinic acid are chemicals that can be produced from lignocellulosic biomass. In this research, mass balance simulation of furfural and levulinic acid production at scale of 100 tons of biomass/year was examined. This research using various models of kinetic reaction and biomass to solvent ratio from lignocellulosic biomass raw materials consisting of cellulose, hemicellulose, lignin, ash, and water composition of 35%, 30%, 25%, 3%, and 7%. The kinetic models used in this research were separate kinetic models and simultaneous model (model-3). The separate kinetic models were divided into two models which separate kinetic model 1 (model-1) and separate kinetic model 2 (model-2). SuperPro Designer 9.0 software was used to calculate mass balance simulation. From the research, it was found that variations in kinetic reaction model affected furfural and levulinic acid production. Higher biomass to solvent ratio produced higher furfural and levulinic acid production. The highest furfural produced from simulation process was kinetic reaction model-2 with a biomass to solvent ratio of 1:30 and 0.67 liter furfural/hour. While the highest levulinic acid produced from the simulation process was kinetic reaction model-1 with a biomass to solvent ratio of 1:30 and 2.37 liter levulinic acid/hour.

Suppression of Interphase Dissolution Via Solvent Molecule Tuning for Sodium Metal Batteries.

Solvent molecule tuning is used to alter the redox potentials of solvents or ion-solvent binding energy for high-voltage or low-temperature electrolytes. Herein, an electrolyte design strategy that effectively suppresses solid electrolyte interphase (SEI) dissolution and passivates highly-reactive metallic Na anode via solvent molecule tuning is proposed. With rationally lengthened phosphate backbones with ─CH2 ─ units, the low-solvation tris(2-ethylhexyl) phosphate (TOP) molecule effectively weakens the solvation ability of carbonate-based electrolytes, reduces the free solvent ratio, and enables an anion-enriched primary Na+ ion solvation sheath. The decreased free solvent and compact lower-solubility interphase established in this electrolyte prevent electrodes from continuous SEI dissolution and parasitic reactions at both room temperature (RT) and high temperature (HT). As a result, the Na/Na3 V2 (PO4 )3 cell with the new electrolyte achieves impressive cycling stability of 95.7% capacity retention after 1800 cycles at 25 °C and 62.1% capacity retention after 700 cycles at 60°C. Moreover, the TOPmolecule not only maintains the nonflammable feature of phosphate but also attains higher thermal stability, which endows the electrolyte with high safety and thermal stability. This design concept for electrolytes offers a promising path to long-cycling and high-safetysodium metal batteries.

Vigna unguiculata L. Walp. Leaves as a Source of Phytochemicals of Dietary Interest: Optimization of Ultrasound-Assisted Extraction and Assessment of Traditional Consumer Habits.

Vigna unguiculata L. Walp. is an African crop spread worldwide mainly for pulses production. Despite being a neglected and under-utilized food, cowpea leaves are a rich source of phytochemicals and micronutrients. The aim of the work is to characterize the phytochemical composition of cowpea leaves by an optimized ultrasound-assisted extraction (USAE) and to compare raw and boiled leaves. A three-level factorial design (Box-Behnken) was employed for the optimization of the USAE considering three different parameters (% ethanol, drug-to-solvent ratio, and number of cycles). The optimized extracts were characterized by LC/MS/MS. Finally, leaves were boiled at 100 °C for 30 min to simulate traditional cooking procedures and compared to raw leaves. The best extraction condition was EtOH/H2 O 1 : 2 v/v, drug to solvent ratio 1 : 47 w/v, and 3 extraction cycles. The phytochemicals identified mainly belong to the family of phenolic acids, flavonoids, terpenoids, and alkaloids. Boiled leaves revealed a significant loss of most phytochemicals and a net decrease of their antioxidant activity compared to the raw ones. The results highlight the potential nutraceutical value of cowpea leaves whilst the impoverishment triggered by traditional consumer habits pushes the need to evaluate alternative cooking procedures helpful in the maintenance of their phytochemical properties.

EXTRACTION OPTIMIZATION AND PHENOLIC COMPOUNDS ANALYSIS IN FICUS CARICA L. FRUITS BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

One of the important tasks of modern pharmacology and pharmacy is the search and development of safe and effective medicines. On the pharmaceutical market of Ukraine, there is a trend of development of organic chemistry and the emergence of new synthetic medicines. However, the search and in-depth study of plant raw materials remains relevant, as medicinal products based on it show low toxicity and have high indicators of biological activity. According to literature sources, ripe fruits of Ficus carica L. of the Moraceae family are a promising object for further research. It is known that the fruits of Ficus carica L. contain a whole complex of biologically active substances that provide them with antioxidant, antiinflammatory, choleretic and antispasmodic effects. The aim of the work was to study the qualitative composition and quantitative content of biologically active compounds of phenolic nature in ripe fruits of Ficus carica L. by the method of high-performance liquid chromatography. The fruits of Ficus carica L. were extracted under different conditions and methods of extraction. Various concentrations of the water-ethanol mixture (30%, 50% and 70%) were chosen as the solvent, with a ratio of solvent to plant material of 1:8 and grinding of the plant material to a size of 5 mm. A series of extractions was carried out in a Soxhlet apparatus and by the maceration method until the target product was completely extracted. The main criterion for evaluating the optimal conditions and extraction method was the quantitative content of phenolic compounds, which was determined spectrophotometrically according to the Folin-Chocalteu method in terms of gallic acid. It was established that the optimal conditions that ensure the maximum extraction of polyphenolic compounds from plant raw materials are the use of 70% alcohol as an extractant when using both extraction methods. It has also been proven that higher rates of target product yield are observed when extracted in a Soxhlet apparatus. Using the method of high-performance liquid chromatography at a wavelength of 225 nm, it was established that the extract of Ficus carica L. contains such groups of phenolic compounds as: phenolic acids (101.4 μg/ml), catechins (98.08 μg/ml), catechin-like substances (599.29 μg/ml), flavanols (1.07 μg/ml), flavonol-like (43.10 μg/ml), flavonoids (99.15 μg/ml). The total content of polyphenolic compounds in the studied sample of the extract from the fruits of Ficus carica L. is 1420.28 μg/ml, where the share of unidentified compounds is 478.19 μg/ml.

Structural Variants and Ultralow Detection Ability for Tryptamine in Two Polymorphs of a Zincophosphite Framework.

Two organic-inorganic hybrid zinc phosphites incorporating 1,2,4,5-tetrakis(imidazol-1-ylmethyl)benzene (TIMB) molecules were synthesized under hydro(solvo)thermal methods and structurally characterized by single-crystal X-ray diffraction (SCXD). Interestingly, the solvent ratio of water to dimethylformamide induced the formation of a new compound of Zn2(TIMB)0.5(HPO3)2·3H2O (1) and our previously reported structure of Zn2(TIMB)0.5(HPO3)2·H2O (2). Additionally, their dehydrated crystals (1a and 2a) were prepared through heat treatment at 150 °C. SCXD and powder X-ray diffraction showed that all four compounds share the same framework formula of Zn2(TIMB)0.5(HPO3)2 but exhibit a huge difference in their inorganic components and final structures. In 1 and 1a, the inorganic units formed two-dimensional zincophosphite layers, while in 2 and 2a, they formed one-dimensional chains. The inorganic parts of 1 (1a) and 2 (2a) were bridged with TIMB linkers, resulting in 3D structures with rectangular and tubular windows, respectively. Furthermore, 1 was coated on the screen-printed carbon electron as a hybrid material, displaying excellent performance while having a linear relationship with an R2 value of 0.99 within the concentration range of 10-10 to 10-6 mol/L for detecting tryptamine (Try) molecules. Moreover, the results showed that 1 exhibits an ultralow limit of detection of 5.43 × 10-11 mol/L and high specificity toward Try over histamine, ascorbic acid, uric acid, and glucose. The synthesis, structural diversity, stability, and sensing ability are also discussed.

Reverse Micellar Dyeing of Cotton Fabric with Reactive Dye Using Biodegradable Non-Ionic Surfactant as Nanoscale Carrier: An Optimisation Study by One-Factor-at-One-Time Approach.

This study investigates the feasibility of using biodegradable secondary alcohol ethoxylate (SAE) non-ionic surfactant as a building block for the formation of reverse micelles, functioning as reactive dye carriers for the dyeing of cotton fabric in non-aqueous octane medium. Ten dyeing parameters were optimised, by a one-factor-at-a-time approach, namely: (i) effect of colour fixation agent; (ii) surfactant-to-water mole ratio; (iii) surfactant-to-co-surfactant mole ratio; (iv) volume of soda ash; (v) volume of dye; (vi) solvent-to-cotton ratio; (vii) dyeing temperature; (viii) dyeing time; (ix) fixation time; (x) soda-ash-to-cotton ratio. The colour properties, fastness properties and physical properties of SAE-dyed samples were experimentally compared with the conventional water-dyed samples. The optimised condition was found when SAE samples were dyed as follows: (a) 1:20 surfactant-to-water ratio; (b) 1:8 surfactant-to-co-surfactant ratio; (c) 10:1 solvent ratio; (d) 40 min dyeing time; (e) 60 min fixation time; and (f) 70 °C dyeing and fixation temperature. The results showed that SAE-dyed samples have better colour strength, lower reflectance percentage and comparable levelness, fastness and physical properties than that of water-dyed samples. SEM images revealed that the dyed cotton fibres had no severe surface damage caused by an SAE-based reverse micellar dyeing system. The TEM image depicts that the reverse micelle was of nanoscale, spherical-shaped and had a core-shell structure, validating the presence of reverse micelle as a reactive dye carrier and the potential of an SAE-based reverse micellar system for dyeing of cotton fabrics.

High-performance electrospun polystyrene-based nanofiber membrane for efficient SO2 capture

It is essential to design a stable membrane material to solve the pollution produced by SO2 emissions. This study aims to fabricate polystyrene (PS) nanofiber membranes, which are applied for flue gas desulfurization. PS nanofiber membranes are fabricated via electrospinning with porous polypropylene (PP) membrane as the support and high hydrophobic PS as the main membrane material. The modified membranes are characterized by scanning electron microscopy, true color confocal microscopy and other analyticalmethods, and the effects of mixed solvent ratio and polymer concentration on the desulfurization performance and on the stability of PS nanofiber membranes are investigated. The results suggest that an optimum hydrophobicity of PS nanofiber membrane is obtained with a water contact angle of 145°, when the polymer concentration is 5 %. The average pore size of PS nanofiber membrane is 1.56 μm, and the liquid entry pressure of water (LEPw) is 0.26 bar and the roughness of membrane is 5.674 μm. The desulfurization performance of the PS nanofiber membrane is better than that of the PP membrane. The SO2 absorption flux of the modified membranes keeps at 7.2 × 10−4 to 7.6 × 10−4 mol·m−2·s−1 during 5 h operating, and SO2 removal efficiency is up to 50 %, which potentially makes contributions to air pollution reduction.

Molecular Networking and Bioassay-Guided Preparation and Separation of Active Extract and Constituents from Vicia tenuifolia Roth.

Molecular networking drove the selection of material from V. tenuifolia organs that targeted active flavonoid glycosides. To optimize the extraction process, the flowers of V. tenuifolia were used to produce an anti-inflammatory extract. The effects of variables-organic solvent ratio; extraction time; and temperature-were investigated by the response of anti-inflammatory activity. Bioactivities-guided experiments helped identify fractions with high total phenolic and flavonoid content as well as antioxidant potential. Furthermore, one new compound (1), 19 first isolated together, and two known compounds were obtained and identified from the active fraction of this plant. Among them, compounds (15 and 22) were first reported for nuclear magnetic resonance (NMR) data from this study. All the isolates were evaluated for their anti-inflammatory capacity throughout, modulating nitric oxide (NO), interleukin (IL)-1β, and IL-8 production. Active compounds were further investigated for their regulation and binding affinity to the inducible nitric oxide synthase (iNOS) and cyclooxygenase-2 (COX-2) proteins by Western blot and in silico approaches, respectively. The findings of this study suggested that the developed extract method, active fraction, and pure components should be further investigated as promising candidates for treating inflammation and oxidation.

Extraction of triterpene acids from loquat leaves via a novel hydrophobic deep eutectic solvent screened by COSMO-SAC model

Triterpene acids (TTAs) have promising applications in functional food, medicine and other fields. Here, ultrasonic-assisted hydrophobic deep eutectic solvent (HDES) extraction was employed to gain TTAs from loquat leaves. Combining COSMO-SAC model prediction with experimental verification，the HDES, composed of thymol and benzyl alcohol (molar ratio 2:1), was proved to have the highest extraction ability for TTAs. The preliminarily optimized extraction conditions were solid to solvent ratio 1:10 (g/g), temperature 60 °C and extraction time 60 min. Under these conditions, the extraction yield of ursolic acid (the main component of loquat leaf TTAs) was 17.769 ± 0.799 mg/g dry loquat leaf. HDES and TTAs were recovered from HDES extracting solution via gradient elution (60% and 80% ethanol aqueous solution, respectively) based on C18 reverse-phase silica gel column chromatography under low pressure (0.5 MPa). Recovered HDES could be reused for extracting TTAs from loquat leaves directly and had a similar extraction performance compared to fresh HDES. The purity of the obtained crude TTAs sample was 81.18% based on the total contents of maslinic acid (MA), corosolic acid (CA), oleanolic acid (OA) and ursolic acid (UA), with a mass ratio of 11:26:10:53. Crude TTAs sample was further separated by C18 reverse-phase silica gel column chromatography using 80% ethanol aqueous solution as mobile phase under high pressure (15 Mpa). By this mean, CA sample with 69.30% purity (MA to CA mass ratio 7:18) and UA sample with 93.94% purity (OA to UA mass ratio 4:21) were obtained. The in vitro antioxidant ability order of the attained TTAs samples was CA sample > crude TTAs sample > UA sample. This study laid a good scientific basis for applying HDES and C18 reverse-phase silica gel column chromatography in the bioactive component extraction and separation fields. It also provided theoretical basis and technical support for obtainment and utilization of high-purity loquat leaf TTAs in the fields of medicine, functional food, cosmetics and so on.