Comparison of conventional and ultrasound-assisted extraction of phenolics-rich heteroxylans from wheat bran

Various two-step extraction procedures with and without a short application of ultrasound in the first step at various reaction conditions (extracting agent, temperature and time), and constant conditions in the second step (5% NaOH, room temperature, 60 min) were used to isolate the hemicellulose component of industrial wheat bran. The polysaccharides recovered from the extracts were characterised by yield, chemical composition and radical scavenging activity. Similar total yields of polysaccharides were achieved by a short ultrasound-assisted extraction (up to 10 min) in the first step using 0.5% or 2% NaOH, when compared to the classical extraction lasting 60 min, what represents a shortening of the process by about 60% and lower consumption of the NaOH. The extracted polysaccharides comprised a complex of phenolics-rich heteroxylans contaminated to various extents with co-extracted amylose-rich starch as well as protein, which can be in part governed by the extraction conditions. The water-soluble fractions from both the classical and ultrasonics experiments were shown to exhibit significant radical scavenging activity in vitro, indicating their potential application as polysaccharide-based antioxidants.     

超声波强化提取对茯苓水溶性多糖结构影响的研究

以茯苓菌核为原料,采用正交实验法确定超声波辅助热水浸提茯苓水溶性多糖的最佳提取条件,并对超声波辅助提取中药多糖的机理进行初步研究。用苯酚硫酸法测定糖含量,傅立叶变换红外光谱仪(FTIR)分析糖类官能团,气相色谱法测定单糖组成,原子力显微镜观察多糖结构,并将测定结果与传统热水法浸提所得茯苓多糖进行对比。实验结果表明:采用超声波辅助热水浸提可以使水溶性茯苓多糖的提取率达到2.71%(传统热水浸提法提取率为1.49%),传统热水浸提得茯苓多糖(PPTH)与超声波辅助热水浸提得茯苓多糖(PPUH)具有相同的单糖组成,都包含核糖、木糖、甘露糖、果糖、半乳糖和葡萄糖,二者的红外吸收谱也基本相同,原子力显微镜扫描分析显示,PPTH整体呈现网状结构,而PPUH主要以长短不一的近棒状结构存在。     

Ultrasound-assisted extraction and characteristics of maize polysaccharides from different sites

Antitumor, antioxidant, hypoglycemic, and immunomodulatory properties are all exhibited by maize polysaccharides. With the increasing sophistication of maize polysaccharide extraction methods, enzymatic method is no longer limited to a single enzyme to extract polysaccharides, and is more often used in combination with ultrasound or microwave, or combination with different enzymes. Ultrasound has a good cell wall-breaking effect, making it easier to dislodge lignin and hemicellulose from the cellulose surface of the maize husk. The “water extraction and alcohol precipitation” method is the simplest but most resource- and time-consuming process. However, the “ultrasound-assisted extraction” and “microwave-assisted extraction” methods not only compensate for the shortcoming, but also increase the extraction rate. Herein, the preparation, structural analysis, and activities of maize polysaccharides were analyzed and discussed.     

Ultrasound-assisted extraction of water-soluble polysaccharides from the roots of valerian (Valeriana officinalis L.)

The insoluble plant residues, obtained after preparation of medicinal tinctures from the roots of valerian (Valeriana officinalis L.) by classical and ultrasound-assisted extraction with aqueous ethanol in a pilot plant, were subsequently treated with hot water to isolate the accessible polysaccharide cell wall components. At almost equal amounts of the hot-water extractable material, the yields of the recovered polysaccharides were lower in the ultrasonical experiment. This is due to the fact that a part of accessible polysaccharides were already solubilised by the aqueous ethanol and recoverable from the medicinal tincture. Therefore, the net yield of extracted polysaccharides was enhanced in the ultrasonical procedure. This fact as well as the sugar composition and structural features of the isolated polysaccharides suggest that ultrasonication have attacked the integrity of cell walls, released and degraded its most accessible polysaccharides (pectic polysaccharides and starch) and increased also the extractibility of its less accessible components--xylan, mannan and glucan. The water-soluble polysaccharide fractions from both the conventional and ultrasonical experiments exhibit significant immunostimulatory activities in mitogenic and comitogenic thymocyte tests.     

Ultrasound-assisted extraction and analysis of maidenhairtree polysaccharides

The maidenhairtree polysaccharides (MTPs) have important application prospects. So, the extraction, purification, structure, derivatization and biological activities of polysaccharides from leaves, fruits, and testae of maidenhairtree were disscussed. Polysaccharides were extracted by collaborative extraction methods such as ultrasound-assisted extraction and microwave-assisted extraction. The ultrasound-assisted extraction had higher content and higher efficiency. The structural characteristics and structure-activity relationship of maidenhairtree polysaccharides were studied in order to provide theoretical basis and technical support for the further development and utilization of maidenhairtree polysaccharides.     

Comparison of classical and ultrasound-assisted extraction of polysaccharides from Salvia officinalis L

After preparation of medicine tinctures from the herbal plant Salvia officinalis by classical and ultrasound-assisted extraction with aqueous ethanol, the insoluble plant residues were subsequently treated with hot water and dilute alkali to isolate polysaccharide cell wall components. The yields of the hot water extract as well as total extracted polysaccharides were higher in the case of the ultrasound-treated plant in both laboratory and pilot plant experiments. The water-extractable polysaccharide fractions, in all cases, contained glucose, galactose and arabinose as main sugar components, whereas the alkali-extractable fractions were rich in xylans. The fractions also contained considerable amounts of proteins. The water-soluble polysaccharides may contribute to the biological activity of the plant decoction. The results indicate that the addition of a subsequent extraction step during the preparation of the herbal tincture might contribute to a better exploitation of the raw material.     

Ultrasound-assisted extraction and properties of polysaccharide from Ginkgo biloba leaves

Response surface methodology (RSM) was used to optimize the ultrasound-assisted extraction conditions of Ginkgo biloba leaves polysaccharide (GBLP). The optimum extraction conditions for the ultrasound-assisted extraction of GBLP were obtained as liquid to material ratio of 30 mL/g, ultrasonic power of 340 W, and extraction time of 50 min. Under these conditions, the yield of GBLP was 5.37 %. Two chemically modified polysaccharides, CM-GBLP and Ac-GBLP, were obtained by carboxymethylation and acetylation of GBLP. The physicochemical properties of these three polysaccharides were comparatively studied and their in vitro antioxidant activities were evaluated comprehensively. The results showed that the solubility of the chemically modified polysaccharides was significantly enhanced and the in vitro antioxidant activity was somewhat improved. This suggests that carboxymethylation and acetylation are effective methods to enhance polysaccharide properties, but the results exhibited some uncontrollability. At the same time, GBLP has also shown high potential for research and application.     

Ultrasound-assisted extraction of polysaccharides from Rhododendron aganniphum: Antioxidant activity and rheological properties

In this study, we aimed to optimize the extraction of polysaccharides from the leaves of Rhododendron aganniphum and investigate its rheological properties and antioxidant activity. After optimizing the operating parameters using a Box-Behnken design (BBD), the results showed that the optimal ultrasound-assisted extraction conditions were as follows: extraction temperature, 55 °C; liquid-solid ratio, 25:1; extraction time, 2.2 h; and ultrasound treatment power, 200 W. The optimized experimental yield of polysaccharides by ultrasound-assisted extraction (PUAE) was 9.428%, higher than that obtained by hot water extraction (PHWE) for 12 h at the same liquid-solid ratio and extraction temperature. In the in vitro antioxidant activity tests, PUAE had higher positive radical scavenging activity for hydroxyl, superoxide and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radicals than PHWE. However, PUAE and PHWE solutions had similar intermolecular interactions in the steady-shear flow and dynamic viscoelasticity tests, resulting in similar macroscopic behaviour. With respect to the apparent viscosity, storage modulus (G′) and loss modulus (G″) of PUAE were lower at the same shear rate or angular frequency. All PUAE solutions exhibited non-Newtonian shear-thinning pseudoplastic behaviour that was accurately described by the Carreau model but was better fit by the power-law model at high shear rates (≥1/s), which demonstrated that the variation in the apparent viscosity dependence was greater at higher concentrations and shear rates. The G′ and G″ of the solutions increased as the experimental frequency increased from 0.05 to 500 rad/s under all experimental concentrations, and the modulus crossover point decreased gradually with increasing PUAE concentration. The above results demonstrated that the ultrasound-assisted extraction methods gave a higher yield of polysaccharides from the leaves of R. aganniphum with a shorter extraction time than the hot water extraction method, which could affect the apparent viscosity and dynamic viscoelasticity. PUAE presented good radical scavenging activity for DPPH, superoxide and hydroxyl radicals in vitro and could be used as a natural antioxidant in the food and medical industries.     

Continuous and pulsed ultrasound-assisted extractions of antioxidants from pomegranate peel

There is a great demand for developing efficient extraction methods in order to reduce extraction time and increase the yield and activity of functional antioxidants. The yields, activities, and extraction kinetics of antioxidants from dry peel of pomegranate marc were studied using ultrasound-assisted extraction in continuous and pulsed modes and the results were compared with conventional extraction (CE) at a temperature of 25±2°C and water/peel ratio of 50/1, w/w. The studied factors were intensity level and treatment time for continuous ultrasound-assisted extraction (CUAE), and intensity level, number of pulse repetition, and pulse duration and interval for pulsed ultrasound-assisted extraction (PUAE). The results showed that all factors significantly affected the antioxidant yield, but only treatment time had a significant effect on the antioxidant activity. Compared to CE, PUAE at intensity level of 59.2 W/cm(2), and the 5 and 5s of pulse duration and interval increased the antioxidant yield by 22% and reduced the extraction time by 87%. Similarly, CUAE at the same intensity level increased the antioxidant yield by 24% and reduced the extraction time by 90%. Since PUAE had 50% energy saving compared to CUAE, we recommend using PUAE for the extraction with antioxidant yield of 14.5% and DPPH scavenging activity of 5.8 g/g. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound-assisted extractions under PUAE and CUAE. This research clearly demonstrated the superiority of PUAE for producing antioxidants from peel of pomegranate marc.     

Continuous and pulsed ultrasound-assisted extractions of antioxidants from pomegranate peel

There is a great demand for developing efficient extraction methods in order to reduce extraction time and increase the yield and activity of functional antioxidants. The yields, activities, and extraction kinetics of antioxidants from the dry peel of pomegranate marc were studied using ultrasound-assisted extraction in continuous and pulsed modes and the results were compared with conventional extraction (CE) at a temperature of 25 ± 2 °C and water/peel ratio of 50/1, w/w. The studied factors were intensity level and treatment time for continuous ultrasound-assisted extraction (CUAE), and intensity level, number of pulse repetition, and pulse duration and interval for pulsed ultrasound-assisted extraction (PUAE). The results showed that all factors significantly affected the antioxidant yield, but only treatment time had a significant effect on the antioxidant activity. Compared to CE, PUAE at an intensity level of 59.2 W/cm², and a pulse duration of 5 s and a resting interval of 5 s increased the antioxidant yield by 22% and reduced the extraction time by 87%. Similarly, CUAE at the same intensity level increased the antioxidant yield by 24% and reduced the extraction time by 90%. Since PUAE had 50% energy saving compared to CUAE, we recommend using PUAE for the extraction with antioxidant yield of 14.5% and DPPH scavenging activity of 5.8 g/g. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound-assisted extractions under PUAE and CUAE. This research clearly demonstrated the superiority of PUAE for producing antioxidants from peel of pomegranate marc.     

Effect of ultrasound on the extractibility of corn bran hemicelluloses

Various two-step extraction procedures with and without a short application of ultrasound in the first step were used to examine the effect of sonication on the extractibility and properties of the non-cellulose components of industrial corn bran (CB). The polysaccharides recovered from the extracts of the first (FI) and second (FII) extraction step were characterised by yield and composition. Using water as extractant in the first step, similar yields of total extracted polysaccharides (FI + FII) were obtained by the short sonication treatment when compared to the classical procedures using H2O2-containing alkaline media in the first step. The yields of FI + FII showed a substantial increase (10-40%) after application of ultrasound in 1% and 5% NaOH in comparison to those of the classical procedures. The content of the neutral sugar components constituting the CB xylan varied from 65 to 88 mol% in dependence on the conditions used in the first extraction step.     

Ultrasound-assisted extraction of xyloglucan from apple pomace

Ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction method for the isolation of xyloglucan from apple pomace. The apple pomace samples were extracted under indirect sonication in an ultrasound cleaning bath. The ultrasound extraction was compared with the conventional method, on the productions of xyloglucan. It was found that the ultrasound-assisted extraction of xyloglucan was about three times faster than the traditional extraction method. Response surface methodology was employed to study the effect of liquid:solid ratio, KOH concentration and ultrasound-assisted extraction time on the yield of xyloglucan from apple pomace. Regression analysis was performed on the data obtained. The most relevant variable was the quadratic of liquid:solid ratio. The coefficient determination (R²) was good for the second-order model. The optimum combination was determined as a liquid:solid ratio of 34.4:1 (v/w), a KOH concentration of 3.3 M and an ultrasound-assisted extraction time of 2.5 h.     

Ultrasound-assisted extraction of phillyrin from Forsythia suspensa

Forsythia suspensa (Thunb.) Vahl is one of the most widely used traditional Chinese medicines, and possesses important biological activities, such as antibacterial, antiviral, anti-inflammatory and antioxidant activities. Phillyrin is the main bioactive component of Forsythia suspensa. In this paper, ultrasound-assisted extraction of phillyrin from Forsythia suspensa was studied with HPLC-photodiode array detection. Effects of several experimental parameters, such as type and concentration of extracting solvent, ratio of liquid to material, extraction temperature, and time of sonication on extraction efficiencies of phillyrin from Forsythia suspensa were evaluated. The optimal extraction conditions were 1g plant sample with 10 ml of 20% methanol and the extraction for 60 min at 60°C under ultrasonic irradiation. Under the optimum conditions, the yield of phillyrin was 0.713±0.009 mg/g. The results indicated that the ultrasound-assisted extraction is a very useful method for the extraction of important phytochemicals from plant materials.     

Green ultrasound-assisted extraction of carotenoids from pomegranate wastes using vegetable oils

The objective of this work was to develop a new process for pomegranate peels application in food industries based on ultrasound-assisted extraction of carotenoids using different vegetable oils as solvents. In this way, an oil enriched with antioxidants is produced. Sunflower oil and soy oil were used as alternative solvents and the effects of various parameters on extraction yield were studied. Extraction temperature, solid/oil ratio, amplitude level, and extraction time were the factors investigated with respect to extraction yield. Comparative studies between ultrasound-assisted and conventional solvent extraction were carried out in terms of processing procedure and total carotenoids content. The efficient extraction period for achieving maximum yield of pomegranate peel carotenoids was about 30 min. The optimum operating conditions were found to be: extraction temperature, 51.5 °C; peels/solvent ratio, 0.10; amplitude level, 58.8%; solvent, sunflower oil. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound extraction under different processing parameters.     

Investigation on ultrasound-assisted extraction of salvianolic acid B from Salvia miltiorrhiza root

It is reported that salvianolic acid B, a bioactive phenolic compound contained in the root of Salvia miltiorrhiza, exhibits a much stronger activity in free radical scavenging and antioxidance than those of vitamin E. When a conventional refluxing method is adopted to extract salvianolic acid B from the root, in which the materials are subjected to higher temperature and longer time, the yield of this phenolic compound is lower due to the possibility of its hydrolysis to tanshinol. However, a higher extraction yield can be achieved over a shorter time period and lower temperature when an ultrasound-assisted extraction method is used. This paper investigated the parameters influencing the extraction of salvianolic acid B. Factors such as extraction time, frequency of the ultrasound, the ratio of solvent to material, and types of extraction solvent were examined. A comparison was also conducted between conventional refluxing and ultrasound-assisted extraction. Results showed that the optimal parameters to extract salvianolic acid B from the root of S. miltiorrhiza were as follows: ultrasonic frequency: 45 Hz; solvent: 60% aqueous ethanol; extraction temperature: 30 °C; extraction time duration: 25 min.; ratio of solvent to material: 20:1 (v/w, ml/g). Under these conditions, the yield of salvianolic acid B was 5.17 mg/g (33.93 mg/g) higher than those with conventional refluxing method (28.76 mg/g), indicating that the efficiency and the yield of ultrasound-assisted extraction method are higher than reflux method, and the hydrolysis of salvianolic acid B to tanshinol is effectively avoided.     

Artificial neural network model- and response surface methodology-based optimization of Atractylodis Macrocephalae Rhizoma polysaccharide extraction,kinetic modelling and structural characterization

Atractylodis Macrocephalae Rhizoma (AMR) is the dried rhizome of Atractylodes macrocephala Koidz, which is widely used in the development of health products. AMR contains a large number of polysaccharides, but at present there are fewer applications for these polysaccharides. In this study, the effects of different extraction methods on the Atractylodis Macrocephalae Rhizoma polysaccharide (AMRP) yield were investigated, and the conditions for ultrasound-assisted extraction were optimized by response surface methodology (RSM) and three neural network models (BP neural network, GA-BP neural network and ACO-GA-BP neural network). The best conditions were a liquid-to-solid ratio of 17 mL/g, ultrasonic power of 400 W, extraction temperature of 72 °C, and extraction time of 40 min, which yielded 31.31% AMRP. The kinetic equation of AMRP was determined and compared with the results predicted by three neural network models. It was finally determined that the extraction conditions, kinetic processes and kinetic equation predicted by the GA-ACO-BP neural network were optimal. In addition, AMRP was characterized using SEM, FTIR, HPLC, UV, XRD, and NMR, and the structural study revealed that AMRP has a rough exterior and a porous interior; moreover, it contains high levels of glucose (5.07%), arabinose (0.80%), and galactose (0.74%). AMRP has three crystal structures, consisting of two β-type monosaccharides and one α-type monosaccharide. Additionally, the effectiveness of AMRP as an antioxidant was demonstrated in an in vitro experiment.     

Quantitative determination of oil content in small quantity of oilseed rape by ultrasound-assisted extraction combined with gas chromatography

Accurately quantitative determination of oil content in oilseed rape plays an important role in varieties breeding for improving oil content in seeds. However, large quantity of oilseeds were needed in order to obtain accuracy and precision results by using standard Soxhlet extraction method, which may be a handicap in analysis of small, rare and precious samples in plant breeding. In the present work, ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction method for the isolation of oil from small quantity of oilseed rape (<20 mg). The oil of oilseed rape samples was extracted by ultrasound-assisted method, and then the fatty acids and total oil content of the seeds were qualitatively and quantitatively determined by gas chromatography (GC). Extraction efficiency of total oil obtained by ultrasound-assisted extraction through an orthogonal experiment (L(9) (3(4))) were investigated to get the best extraction conditions. Statistical analysis showed that the variable with the largest effect was the ultrasound-assisted extraction time which was followed by the ultrasound-assisted extraction power, and the liquid:solid ratio. A liquid:solid ratio of 1:4 (L:g), an ultrasound-assisted extraction time of 60 min and an ultrasound-assisted extraction power of 500 W were found to be optimal for oil extraction from oilseed rape. By comparing with the conventional method, it was found that the ultrasound-assisted extraction of oil from oilseed rape was about five times faster than the traditional extraction method. By the use of ultrasound-assisted extraction combined with GC analysis, the fatty acids and total oil content in small quantity of seeds (<20 mg) were successfully qualitatively determined and the results are in agreement with that obtained by traditional standard method.     

Ultrasound induced green solvent extraction of oil from oleaginous seeds

Ultrasound-assisted extraction of rapeseed oil was investigated and compared with conventional extraction for energy efficiency, throughput time, extraction yield, cleanness, processing cost and product quality. A multivariate study enabled us to define optimal parameters (7.7 W/cm² for ultrasonic power intensity, 40 °C for processing temperature, and a solid/liquid ratio of 1/15) for ultrasound-assisted extraction of oil from oilseeds to maximize lipid yield while reducing solvent consumption and extraction time using response surface methodology (RSM) with a three-variable central composite design (CCD). A significant difference in oil quality was noted under the conditions of the initial ultrasound extraction, which was later avoided using ultrasound in the absence of oxygen. Three concepts of multistage cross-current extraction were investigated and compared: conventional multistage maceration, ultrasound-assisted maceration and a combination, to assess the positive impact of using ultrasound on the seed oil extraction process. The study concludes that ultrasound-assisted extraction of oil is likely to reduce both economic and ecological impacts of the process in the fat and oil industry.     

均匀设计法优化超声波辅助提取枸杞多糖的工艺

实验采用超声波辅助技术提取枸杞多糖,并通过均匀设计法研究了液料比、提取时间、提取温度和超声功率对枸杞多糖提取的影响.枸杞多糖超声提取的最佳工艺为:液料比21mL/g,提取时间27min,提取温度63℃,超声功率200W,在该条件下枸杞多糖得率为5.16％,且表现稳定.均匀设计法在优化枸杞多糖提取条件中应用效果良好.     

Optimization of ultrasound-assisted extraction of anthocyanins in red raspberries and identification of anthocyanins in extract using high-performance liquid chromatography-mass spectrometry

Anthocyanins (Acys) are naturally occurring compounds that impart color to fruit, vegetables and plants. The extraction of Acys from red raspberry (Rubus idaeus L. var. Heritage) by ultrasound-assisted process (UAP) was studied. A central composite rotate design (CCRD) was used to obtain the optimal conditions of ultrasound-assisted extraction (UAE), and the effects of operating conditions, such as the ratio of solvents to materials, ultrasonic power and extraction time, on the extraction yield of Acys were studied through response surface methodology (RSM). The optimized conditions of UAE were as follows: ratio of solvents to materials was 4:1 (ml/g), extraction time was 200 s, and ultrasonic power was 400 W. Under these conditions 34.5 mg of Acys from 100 g of fresh fruits (T_Acy, expressed as cyanidin-3-glucoside), approximately 78.13% of the total red pigments, could be obtained by UAE. The Acys compositions of extracts were identified by high-performance liquid chromatography–mass spectrometry (HPLC–MS), 12 kinds of Acys had been detected and eight kinds of Acys were characterized. Result indicated that cyanidin-3-sophoroside, cyanidin-3-(2^G-glucosylrutinoside), cyanidin-3-sambubioside, cyanidin-3-rutinoside, cyanidin-3-xylosylrutinoside, cyanidin-3-(2^G-glucosylrutinoside), and cyanidin-3-rutinoside were main components in extracts. In addition, in comparison with the conventional solvent extraction, UAE is more efficient and rapid to extract Acys from red raspberry, due to the strong disruption of fruit tissue structure under ultrasonic acoustic cavitation, which had been observed with the scanning electron microscopy (SEM). However, the Acys compositions in extracts by both methods were similar, which were investigated using HPLC profile.