Mechanochemical-assisted Extraction Research Articles

Sustainable Mechanochemical-Assisted Extraction of Active Saponins from Plants with Solid Acid and Alkalis

Sustainable Mechanochemical-Assisted Extraction of Active Saponins from Plants with Solid Acid and Alkalis

Mechanochemical-Assisted Extraction and Biological Activity Research of Phenolic Compounds from Lotus Seedpod (Receptaculum Nelumbinis).

To explore the feasibility of the mechanochemical-assisted extraction (MCAE) of phenolic compounds from lotus seedpod (Receptaculum Nelumbinis), a single-factor experiment combined with response-surface methodology (RSM) was used to optimize the extraction process. The results showed the optimal extraction conditions as follows: Li2CO3 as a solid reagent (25%), an extraction time of 80 min, liquid/solid ratio of 42.8 mL/g, and extraction temperature of 80.7 °C; and the maximum value of total phenolic content (TPC) was 106.15 ± 1.44 gallic acid equivalents (GAE)/g dry weight (DW). Additionally, the 2,2-Diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azinobis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), and ferric reducing antioxidant power (FRAP) were 279.75 ± 18.71, 618.60 ± 2.70, and 634.14 ± 7.17 µmol TE/g, respectively. Ultra-high pressure liquid chromatography combined with triple-time-of-flight mass spectrophotometry (UPLC-Triple-TOF/MS) analysis identified eight phenolic compounds mainly consisting of polyphenols and flavonoids. Moreover, the phenolic compounds showed potent inhibitory effects on both α-amylase and α-glucosidase, with inhibition rates of over 80%. Furthermore, the results showed different degrees of inhibition activity against Bacillus subtilis, Staphylococcus aureus, and Escherichia coli, among which the inhibitory effect on the growth of B. subtilis was the best. This paper shows that the phenolic compounds have good biological activities, which provides a reference for the further exploitation of LSP.

Mechanochemical-assisted extraction and enzymatic hydrolysis of calcium phytate from defatted rice bran

BackgroundMechanochemical-assisted extraction (MCAE) and mechanochemical-assisted enzyme catalysis (MCAEC) methods were developed for extraction and enzymatic hydrolysis of calcium phytate from defatted rice bran, respectively.ResultsThe MCAE conditions were optimized by response surface methodology: 10% sodium carbonate as the solid reagent, 33 min grinding time, 18:1 ball–material ratio, 330 rpm ball milling speed, and pH 5.5 extraction. Under these conditions, the yield of calcium phytate was 97.0 mg/g. The MCAEC conditions were optimized as follows: 2% enzyme addition, MM400 milling time 36 min, PM400 milling speed 262 rpm, MM400 milling frequency 27 Hz, and the addition of pH 5.5 sodium acetate buffer 3 mL. Under these conditions, the hydrolysis rate of calcium phytate was 39.7%.ConclusionCompared with traditional extraction and enzymatic hydrolysis methods, MCAE and MCAEC could obtain higher yields and hydrolysis rates, respectively.Graphical

Mechanochemical-assisted extraction of essential oils from Citrus aurantium L. var. amara Engl.

Mechanochemistry is a process that could convert mechanical energy into the substance's internal energy to induce changes. In the current study, mechanochemistry was employed for the first time to extract the essential oil from Citrus aurantium L. var. amara Engl. Materials and reagents were ground at high speed in a planetary ball mill and exposed to solvent extraction. To achieve the best extraction from Citrus aurantium L. var. amara Engl., the following parameters were selected: 5% fumed silica A200 as solid reagent, ball milling at 300 r/min for 10 min and extraction with n-hexane (1 g/5 mL) during 30 min. These settings gave an essential oil yield of 6.60 ± 0.20%. This is 26 times higher than by hydrodistillation (0.25 ± 0.03%) and more than 3 times higher compared to reflux extraction (2.08 ± 0.16%). The extracts obtained by the three approaches were analysed applying GC-MS. A total of 65 components was identified, including 60 by mechanochemical-assisted extraction, 27 by hydrodistillation and 49 by reflux extraction. Furthermore, scanning electron microscopy was used to observe the changes in material surface structure by the effect of mechanochemical-assisted extraction.

Isolation of Laurus nobilis Leaf Polyphenols: A Review on Current Techniques and Future Perspectives.

In recent years, the market demand for products enhanced with ingredients derived from natural products, such as polyphenols, is rapidly increasing. Laurus nobilis L., known as bay, sweet bay, bay laurel, Roman laurel or daphne is an evergreen Mediterranean shrub whose leaves have traditionally been used in cuisines and folk medicine due to their beneficial health effects, which can nowadays be scientifically explained by various biological activities of the leaf extracts. Many of these activities can be attributed to phenolic compounds present in L. nobilis leaves which include flavonoids, phenolic acids, tannins (proanthocyanidins) and lignans. In order to enable efficient industrial utilization of these valuable compounds, it is crucial to establish optimal extraction procedures resulting in the highest yields and quality of the extracts. This paper offers the first systematic review of current literature on the influence of conventional and advanced extraction techniques, including microwave-assisted, ultrasound-assisted, enzyme-assisted, supercritical-CO2 and mechanochemical-assisted extraction on the phenolic content of L. nobilis leaf extracts, allowing more efficient planning of further research and simplifying the steps towards industrial utilization of this plant.

Mechanochemical-assisted extraction of polysaccharides from bamboo leaves and its optimized processing parameters

Mechanochemical-assisted extraction (MCAE) method was applied to the extraction of polysaccharides from the bamboo leaves. The MCAE parameters were investigated via response surface methodology design experiments, the processing conditions were optimized as follows: milling time 30 min, liquid-solid ratio 2:1, extraction time 48 min. Under these conditions, the experimental value of (11.40 ± 0.12)% corresponded with the value predicted by the model and was higher than super fine-grinding extraction (SFGE) of (11.17 ± 0.15)% and heat reflux extraction (HRE) of (10.92 ± 0.17)%. The mechanism of mechanochemical-assisted extraction (MCAE) was discussed based on scanning electron microscope. Compared to HRE, the extraction time was significantly shortened, the water consumption and extraction temperature were also lowered. MCAE is a good choice for the efficient extraction of polysaccharides from bamboo leaves.

Optimization of mechanochemical-assisted extraction of hesperidin from Pericarpium Citri Reticulatae

Mechanochemical-assisted extraction (MCAE) of hesperidin from Pericarpium Citri Reticulatae was investigated in AGO-2 high intensity planetary activator. In order to optimize extraction efficiency, six variables (different kinds of reagents, Na2CO3 content, grinding time, extraction temperature, extraction time, liquid/solid ratio) were varied. Results showed that the optimum MCAE conditions were determined as: Na2CO3 content of 30.0% (w/w), grinding time 20 min, extraction temperature 20 °C, extraction time 10 min, liquid/solid ratio of 80:1 mL/g. Meanwhile, enhancement of solubility was measured. Fourier transform-infrared spectrometer and scanning electron microscope were used to illustrate structure change of hesperidin after mechanochemical pretreatment. With the optimized parameter settings, MCAE with water as solvent gave the highest hesperidin yield while reducing both extraction time and energy costs compared to the heat-reflux and superfine grinding extraction.

Mechanochemical-Assisted Extraction and Hepatoprotective Activity Research of Flavonoids from Sea Buckthorn (Hippophaë rhamnoides L.) Pomaces.

Pomaces of sea buckthorn berry were usually side-products during the processing of juice. Due to a lack of an economical and effective extraction method, it was typically recognized as waste. For the purpose of resource utilization, the mechanochemical-assisted extraction (MCAE) method was applied to develop an ecofriendly extraction method and product with better pharmacology activity. The parameters were investigated through response surface methodology (RSM) design experiments. The processing conditions were optimized as follows: amount of Na2CO3 40%, ball-to-material rate 29:1 g/g, milling speed 410 rpm, milling time 24 min, extraction temperature 25 °C, extraction time 20 min and the solid-to-solution ratio 1:10 g/mL. Under these conditions, the yields of flavonoids from sea buckthorn pomaces were 26.82 ± 0.53 mg/g, which corresponds to an increase of 2 times in comparison with that extracted by the heat reflux extraction method. Meanwhile, the hepatoprotective activity of sea buckthorn pomaces extracts was studied by the liver injury induced by ip injection of tetracycline. Biochemical and histopathological studies showed that biomarkers in serum and liver of nonalcoholic fatty liver disease (NAFLD) mice were significantly ameliorated when sea buckthorn flavonoids extracted by MCAE were used. Altogether, these results demonstrate that, as a green and efficient extraction, MCAE treatment could increase the extraction yield of sea buckthorn flavonoids, meanwhile it could exhibit significant activity of improving liver function. This research provided a new way to use pomaces of sea buckthorn as a functional food. It also has great value on the comprehensive utilization of nature’s resources.

The Separation and Purification of Ellagic Acid from Phyllanthus urinaria L. by a Combined Mechanochemical-Macroporous Resin Adsorption Method

Ellagic acid is a phenolic compound that exhibits both antimutagenic and anticarcinogenic activity in a wide range of assays in vitro and in vivo. It occurs naturally in some foods such as raspberries, strawberries, grapes, and black currants. In this study, a valid and reliable method based on mechanochemical-assisted extraction (MCAE) and macroporous adsorption resin was developed to extract and prepare ellagic acid from Phyllanthus urinaria L. (PUL). The MCAE parameters, acidolysis, and macroporous adsorption resin conditions were investigated. The key MCAE parameters were optimized as follows: the milling time was 5 min, the ball mill speed was 100 rpm, and the ball mill filling rate was 20.9%. Sulfuric acid with a concentration of 0.552 mol/L was applied for the acidolysis with the optimized acidolysis time of 30 min and acidolysis temperature of 40 °C. Additionally, the XDA-8D macroporous resin was chosen for the purification work. Both the static and dynamic adsorption tests were carried out. Under the optimized conditions, the yield of ellagic acid was 10.2 mg/g, and the content was over 97%. This research provided a rapid and efficient method for the preparation of ellagic acid from the cheaply and easily obtained PUL. Meanwhile, it is relatively low-cost work that can provide a technical basis for the comprehensive utilization of PUL.

Mechanochemical-assisted extraction of protein from watermelon seeds with surfactant

Mechanochemical-assisted extraction (MCAE) was first applied to extract total protein from watermelon seeds with grinding medium of surfactant instead of alkaline. The optimal conditions of MCAE, that is, sodium bis(2-ethylhexyl)sulfosuccinate (AOT) concentration of 0.10 mol/L, water content of 20, ionic strength of 0.05 mol/L, aqueous phase pH of 7, solid to liquid ratio of 0.2 g/mL, ball milling speed of 523 rpm and ball milling time of 10.5 min were obtained by response surface methodology. The highest yield (489.967±1.214 mg/g) of watermelon seeds protein (WSP) was obtained under the optimal conditions, which corresponds to an increase of 19.7% in comparison with that extracted by conventional alkaline extraction. When considering the secondary structure of protein by FTIR and SEM analysis, the random coil structure of watermelon seeds protein was obviously increased and protein aggregations were apparent by conventional alkaline extraction, suggesting the denaturation of WSP under relatively alkaline environment and no loss of protein activities with surfactant interactions, thus MCAE with surfactant retained the better quality of WSP. The results indicated that MCAE with surfactant could be a protective and effective method for the extraction of natural oil-seeds protein.

Screening of β-secretase inhibitors from Dendrobii Caulis by covalently enzyme-immobilized magnetic beads coupled with ultra-high-performance liquid chromatography

In the present study, to effectively discover potential β-secretase inhibitors from Dendrobii Caulis, β-secretase was immobilized on magnetic beads via direct covalent connection and coupled with ultra-high-performance liquid chromatography. Mechanochemical-assisted extraction was used to extract active ingredients from Dendrobii Caulis. The main reaction conditions, including screening enzyme inhibitors, were evaluated, and the most important enzyme kinetic parameters were also investigated across the UV–vis spectrophotometer. Five compounds (rutin, scoparone, naringenin, dendrophenol, and erianin) with high binding affinity to magnetic beads were removed from the extract. The results indicated that β-secretase was successfully immobilized and screened out five potential inhibitor compounds by ligand fishing. The lowest IC50 values were noted for rutin (5.437 μM) and erianin (2.039 μM). This is the first report on immobilized β-secretase on magnetic beads for the identification of potential active compounds against Alzheimer's disease from complex biological mixtures.

Mechanochemical-assisted extraction of platycodin D from the roots of Platycodon grandiflorum with solid alkalis

Mechanochemistry is an interdisciplinary science, which refers to chemical and physicochemical reactions generated by the input of high mechanical energy. The mechanochemical pretreatment with solid alkalis was for the first time successfully used prior to water extraction of platycodin D from roots of Platycodon grandiflorum. The factors affecting the efficiency of mechanochemical-assisted extraction were the solid alkaline reagent type, reagent/material ratio, grinding time, extraction time, material/water ratio and acidification pH value. The highest yield of platycodin D via mechanochemical-assisted extraction (7.16 ± 0.14 mg/g) was obtained by grinding samples with NaOH according to 5 % reagent/material ratio for 5 min in a planetary ball mill, extracting with water at room temperature for 20 min, 1: 30 g/mL material/water ratio and acidification pH 3.5. Compared with superfine grinding extraction (3.26 ± 0.12 mg/g) and Soxhlet extraction (4.18 ± 0.11 mg/g), mechanochemical-assisted extraction reduced both extraction time and temperature, and achieved a higher yield of platycodin D. Furthermore, it used water as solvent, which is more environmental friendly and cheaper. The results indicated that mechanochemical-assisted extraction could be an effective method for extraction of natural compounds.

Mechanochemical-Assisted Extraction and Pharmacological Study of Triterpenoids from Antrodia Camphorata

Antrodia camphorata (AC) is a precious medicinal mushroom native to Taiwan and famous for its excellent pharmacological activity. A ball mill assisted mechanochemical extraction method was applied in the extraction of triterpenoids from Antrodia camphorata. Compared with the ethanol hot thermal reflux method, mechanochemical-assisted extraction afforded an increased yield of triterpenoids to 1.82 ± 0.04% under conditions of mixing with 10 WT% NaHCO3, milling for 20 min, and extracting with water and chloroform. Triterpenoids from Antrodia camphorata extracted by the mechanochemical-assisted extraction method (TAEM) resulted in stronger pharmacological activity as compared to that extracted by ethanol (TAEE). HPLC and LC-MS/MS results showed that the mechanochemical method could extract triterpenoids which were barely extracted by ethanol extraction. The results of this study could provide valuable ideas and a basis for the application of the mechanochemical-assisted extraction method in the extraction of triterpenoids from AC.

Mechanochemical-Assisted Extraction of Active Alkaloids from Plant with Solid Acids

In this work, a novel mechanochemical-assisted extraction (MCAE) coupled with the ultra-high performance liquid chromatography (UHPLC) method was developed to extract two alkaloids with solid acids from Stephania tetrandra S. Moore. To further understand the influence of extraction parameters on the MCAE process, the response surface methodology was applied for systematic investigation. The results showed that the highest yield of alkaloids was obtained within 15 min of the total extraction time under the optimal conditions: oxalic acid (20 wt %), grinding plant materials for 5 min, and the liquid/solid ratio of 20 mL/g. Mechanochemical treatment resulted in the destruction of cell walls and increased the total contact surface area due to the smooth surface changing to an open porous structure. Accordingly, the developed extraction method showed advantages of being more ecofriendly, faster, and more efficient than conventional extraction methods. Meanwhile, the extractant was analyzed by UHPLC. The obtain...

Optimization of mechanochemical-assisted extraction and decoloration by resins of polysaccharides from petals of Crocus sativus L

Polysaccharide from petals of Crocus sativus (PPCs) was extracted by mechanochemical-assisted extraction (MCAE) method. The optimization of MCAE conditions was applied by the Response surface methodology. The optimal conditions were as follows: milling for 8.14 min, keeping in the ultrasonic bath at 40 °C with NaOH (0.2 wt %) for 15 min, and the solid/liquid ratio of 1/30 g/mL. Under the conditions, a yield of 28.97% was obtained, which was very consistent with the predicted yield of 29.20%. The decolorization effects of crude PPCs were studied. HPD-100 resin was selected as the decolorizing resin. The optimized dynamic adsorption condition was flow rate of 5.4 BV/hr, volume of 60 mL, temperature of 20 °C, 5 mg/mL PPCs extract. The ratios of decoloration, deproteinization, and polysaccharide recovery were 86.59, 86.60, and 80.54%, respectively. Then the antiproliferative activity of PPCs was assessed by 3H-TdR method on human lung carcinoma A549 cell and breast cancer MCF7 cell. Practical applications Mechanochemical-assisted extraction was applied to extract polysaccharides from petals of Crocus sativus, which was more time-efficient with fewer solvents than traditional extraction methods. In addition, polysaccharides from petals of Crocus sativus demonstrated a promising antiproliferative property, which means that the byproducts of saffron might be a potential natural drug or health food for human lung carcinoma therapeutics.

Mechanochemical-assisted extraction of flavonoids from bamboo (Phyllostachys edulis) leaves

An efficient mechanochemical-assisted extraction of flavonoids from bamboo (Phyllostachys edulis) leaves was developed. The highest recovery of flavonoids was achieved by grinding the leaves with Na2CO3 (12wt.%) and Na2B4O7·10H2O (2wt.%) for 10min, extraction with water at 25°C and liquid/solid ratio of 20mL/g for 15min. It was compared with heat reflux extraction and alkali extraction, both of which yielded lower recoveries of total flavonoids and representative flavonoids. Mechanochemical processing resulted in particle size reduction and intimate contact between the milled materials. Diffusion was enhanced and flavonoids were converted to be more hydrophilic at room temperature, which promoted the progression of subsequent extraction. It showed the advantages of efficiency, no organic solvent consumption and much lower extraction temperature.

Response surface optimization of mechanochemical-assisted extraction of flavonoids and terpene trilactones from Ginkgo leaves

Mechanochemical-assisted extraction (MCAE) method was developed for extraction of flavonoids and terpene trilactones from Ginkgo leaves. The MCAE parameters and the antioxidant activities of Ginkgo biloba extract (GBE) were investigated. Through response surface methodology design experiments, the processing conditions were optimized as follows: amount of solid reagent (NaHCO 3) 21%, milling time 7.5 min, and ratio of solvent to solid 33 mL/g. Under these conditions, the yields of flavonoids and terpene trilactones in GBE were 6.83 mg/g and 1.72 mg/g, respectively. Compared with the heat reflux extraction method, the yields of flavonoids and terpene trilactones are higher, and the extraction time was significantly shortened. What is more, the MCAE method only used water as solvent. GBE of MCAE possessed notable antioxidant activity with IC 50 values of 11.7 and 13.8 μg/mL, respectively.

Mechanochemical-Assisted Extraction and Antioxidant Activities of Kaempferol Glycosides from Camellia oleifera Abel. Meal

A mechanochemical-assisted extraction (MCAE) method was proposed and investigated for the fast extraction of two kaempferol glycosides (kaempferol-3-O-[2-O-β-D-galactopyranosyl-6-O-α-L-rhamnopyranosyl]-β-D-glucopyranoside and kaempferol-3-O-[2-O-β-D-xylopyranosyl-6-O-α-L-rhamnopyranosyl]-β-D-glucopyranoside) from Camellia oleifera Abel. meal. The effects of operating parameters in terms of NaOH content, grinding time, extraction time, and ratio of solution to solid were evaluated by means of response surface methodology (RSM). Under the optimal conditions with a ratio of material to NaOH of 20:1 (g/g), a milling time of 15 min, and a ratio of solution to solid of 20:1 (mL/g) for 60 min, the maximum extraction yields of the two kaempferol glycosides reached 13.34 and 13.83%, respectively. The antioxidant activity of kaempferol glycosides extract was assessed by 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assay and ferric thiocyanate (FTC) assay. Compared with the heat reflux extraction (HRE) method, the yield and the antioxidant activities of the extracts from MCAE with water as solvent were higher and stronger.

Mechanochemical-assisted efficient extraction of rutin from Hibiscus mutabilis L.

Abstract Mechanochemical-assisted extraction (MCAE) technique was developed for the efficient extraction of rutin from Hibiscus mutabilis L. This process was carried out via mechanochemical pretreatment in AGO-2 high intensity planetary mill. Highest yield of rutin was obtained by grinding H. mutabilis with Na2CO3 (15.0 wt.%) and Na2B4O7·10H2O (1.5 wt.%) for 4 min, extraction temperature at 25 °C, total extraction time of 15 min (two cycles of 10 min and 5 min), acidification pH 5.0 and solvent/material ratio of 25 mL/g. Scanning electron microscopy, X-ray powder diffraction and diffuse-reflectance UV–Vis spectrum were applied to identify the physicochemical property changes. These changes mainly included the enhanced diffusivity and water solubility of rutin resulting from the breakage of cell walls and its transformation into a water-soluble salt form by the mechanochemical pretreatment. Compared with heat reflux and superfine grinding extraction, MCAE showed the advantages of efficiency, no organic solvent consumption and much lower extraction temperature. Industrial relevance In this study, mechanochemical-assisted extraction of rutin from H. mutabilis was developed and the physicochemical changes in this process were supervised. Owing to its great potential to transform the target compounds into water-soluble forms, MCAE provided a good alternative for efficient aqueous extraction of bioactive compounds, especially some poorly water-soluble natural products.

Application of Mechanochemical Pretreatment to Aqueous Extraction of Isofraxidin from Eleutherococcus Senticosus

A mechanochemical pretreatment (MCPT) was applied to aqueous extraction of isofraxidin from the Asian herb Eleutherococcus senticosus. Six extraction variables (Na2CO3 content, particle size, solvent, extraction time, liquid/solid ratio, and extraction temperature) were varied in order to optimize extraction efficiency. Optimal extraction was obtained using superfine powdered plant material (D95 ≤ 44 μm) with Na2CO3 content of 2.0% (w/w) and extraction with water (liquid/solid ratio of 20:1, mL/g) for 5 min at 25 °C. The efficiency of mechanochemical-assisted extraction (MCAE) of isofraxidin was compared to that of heat-reflux and superfine grinding extraction. With the optimized parameter settings, MCAE with water as solvent gave the highest isofraxidin yield while reducing both extraction time and energy costs compared to the conventional methods.