Optimization of Microwave-Assisted Extraction of Phenolic Antioxidants from Grape Seeds (Vitis vinifera)

Grape seeds (Vitis vinifera) are rich in phytochemicals that have antioxidant properties. The influence of independent variables such as microwave power (100, 150, and 200 W), extraction time (2, 4, and 6 min), and solvent concentration (30%, 45%, and 60% ethanol) and their interactions on total phenols and the antioxidant activity (1,1-diphenyl-2-picrylhydrazyl (DPPH) and ferric ion reducing antioxidant power (FRAP)) were determined; and the microwave-assisted extraction (MAE) process was optimized using a central composite design. The total phenols that were expressed as gallic acid equivalents (GAE), catechin equivalents (CAT), and tannic acid equivalents (TAE) were significantly influenced by the solvent concentration and the time of extraction. A numerical optimization was carried out to obtain the overall conditions for MAE of phenolic antioxidants from grape seed. The response variables were maximized for 6 min of MAE of grape seed (GS) with 32.6% ethanol at 121 W with a desirability function of 0.947. The predicted extraction yields were 13?±?0.89, 21.6?±?1.59, and 15.9?±?1.32 mg GAE, CAT, and TAE, respectively per gram of GS. The predicted antioxidant activity per gram of dry weight GS was 80.9% for the inhibition of DPPH and 135 μM ascorbic acid equivalents for FRAP test. The predicted response values were significantly correlated with the observed ones as follows: GAE r?=?0.995, CAT r?=?0.990, TAE r?=?0.996, DPPH r?=?0.996, and FRAP r?=?0.996.     

Extraction of caffeine and catechins using microwave-assisted and ultrasonic extraction from green tea leaves: an optimization study by the IV-optimal design

In this research, optimal conditions for extraction of caffeine and polyphenols were established from Iranian green tea leaves. In the first step, caffeine was extracted with efficacy about 86% versed to 4.5% of EGC + EGCG. The EGCG + EGC was extracted from partially decaffeinated green tea leaves through microwave-assisted extraction (MAE) and ultrasound-assisted extraction (USE) with efficiency levels of 95 and 85%, respectively. The best results for the MAE process were obtained with 7.8 min and three number of extraction cycles and for the USE process were as followed: time 57 min, temperature 65 °C, and the number of extraction cycles 3. The total phenol content values at the best conditions of MAE and the USE processes were 125 ± 5 and 96 ± 6 mg gallic acid/g DW. The 50% inhibition (IC₅₀) on 1,1-diphenyl-2-picrylhydrazyl (DPPH) were 56 and 66 mg/g of phenol for the MAE and USE processes.     

Extraction of antioxidants and flavonoids from yuzu (<Emphasis Type="Italic">Citrus junos</Emphasis> Sieb ex Tanaka) peels: a response surface methodology study

In the present investigation, extraction of antioxidants and flavonoids from the peels of yuzu fruit using a single factor experiment and a response surface methodology (RSM) based on central composite design was studied. Four independent variables were evaluated at five levels with total 29 experimental runs, including ethanol concentration (EtOH), ratio of liquid to material (L/S), extraction temperature (T), and extraction time (t). The total phenolic content (TPC), total flavonoids content (TFC), two indicators of antioxidant capacity (FRAP and DPPH), and three individual major flavonoids in yuzu (hesperidin, naringin, and phloretin) served as the response functions. Quadratic polynomial equations were obtained by multiple regression analysis to predict the optimal extraction conditions. The regression analysis showed that >95?% of variations were explained by the models of different responses considered. The responses were significantly influenced by all studied factors. The Multiresponse optimized conditions targeted at maximizing all the responses were found to be EtOH?=?65.550?%; T?=?43.864?°C; t?=?119.673 min; and L/S?=?37.168 ml/g, with a desirability of 0.950. At the optimized conditions, the experimental values of FRAP (964.9?±?23.1 mgTE/g DW), DPPH (453.0?±?5.2 mgTE/g DW), TPC (1161.2?±?25.2 mgGAE/g DW), (TFC393.4?±?mgQE/g DW), hesperidin (337.2?±?4.0 mg/g DW), naringin (244.9?±?1.1 mg/g DW), and phloretin (43.9 mg/g DW) were in a reasonable agreement with the predicted values. The extraction method was applied successfully to extract antioxidants and flavonoids from yuzu peels. It also allows a fast and cost-saving process for extraction of the studied phytochemicals, in addition to improvement of the quantity of the targeted extract.     

Optimization of green extraction methods for cinnamic acid and cinnamaldehyde from Cinnamon (<Emphasis Type="Italic">Cinnamomum cassia</Emphasis>) by response surface methodology

The major compounds of cinnamon are cinnamic acid and cinnamaldehyde, for which the conditions of microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), and reflux extraction (RE) were optimized using response surface methodology for comparing their efficiencies in terms of extraction yield, consumption of time and energy, and CO₂ emission. The results indicated MAE superiority to UAE and RE owing to the highest yield of target compounds (total yield: 0.89%, cinnamic acid: 6.48 mg/100 mL, and cinnamaldehyde: 244.45 mg/100 mL) at optimum MAE conditions: 59% ethanol, 147.5 W microwave power and 3.4 min of extraction time. RE resulted in comparable yields with the highest consumption of time, energy, and solvent, and least CO₂ emission. Therefore, it is concluded that MAE is the most efficient method for green extraction of cinnamic acid and cinnamaldehyde from cinnamon powder compared to UAE and RE.     

Optimisation of microwave‐assisted extraction of phenolic compounds from broccoli and its antioxidant activity

The effect of independent variables of microwave‐assisted extraction (MAE), extraction temperature (50–90 °C), microwave power (100–200 W), solvent concentration (methanol/water, 50–90%, v/v) and extraction time (1–27 min) on total phenolics and flavonoids contents as well as antioxidant activity of broccoli extracts was investigated. Response surface methodology was successfully applied for optimisation and the high correlation of the mathematical model indicated that a quadratic polynomial model could be used for optimisation of investigated responses. Considering the maximum amount of extracted total phenolics, total flavonoids and antioxidant activity expressed as ORAC value, the optimal conditions for all three investigated responses were obtained (temperature ?71.11 °C; microwave power ?167.03 W; solvent concentration ?75.95%; and extraction time 16.34 min), which is in agreement with optimal conditions obtained for each investigated responses. The development of simultaneously MAE methods for total phenolics, total flavonoids and antioxidant activity of broccoli extracts might simplify assessment of broccoli as valuables source of antioxidants.     

枇杷核黄酮类物质微波法提取及对羟自由基清除作用研究

本文对微波法提取枇杷核中黄酮类物质进行了研究，通过单因素及L9（3^4）正交试验，得到最佳工艺条件：m（乙醇溶液）／m（枇杷核）=15，提取功率为296W，时间120s提取3次，50％的乙醇溶液。按此最佳方法总黄酮提取率为1．41％。微波法与传统溶剂提取法比较，具有提取时间短、提取率高等优点。同时研究了该提取物对羟自由基清除作用，黄酮类物质对羟自由基的清除作用呈线性相关，相关系数R^2为0．9865。     

Microwave‐assisted extraction optimised with response surface methodology and antioxidant activity of polyphenols from hawthorn (Crataegus pinnatifida Bge.) fruit

Microwave‐assisted extraction (MAE) of polyphenols from hawthorn (Crataegus pinnatifida Bge.) fruit was investigated, and the best combination of extraction parameters was obtained using response surface methodology (RSM). The optimised procedure was achieved by soaking the sample powder with 83% ethanol for 90 min at solid–liquid ratio of 1–20, and then microwave irradiation for 13 min at power of 440 W. Under this condition, an extraction yield of 23.5% was obtained and the percentage of phenolic compounds in the extract reached 41.2%. The total content of polyphenols in hawthorn fruit was 96.9 ± 4.3 mg gallic acid equivalents per gram of dry weight measured by Folin‐Ciocalteu reagent method, and the main phenolic compounds were determined as procyanidin B₂, epicatechin, chlorogenic acid, procyanidin C₁ and rutin. Biological studies showed that the extract possessed a strong inhibitory effect against DPPH, hydroxyl radicals and lipid peroxidation, as well as strong reducing power.     

微波和超声波提取脐橙皮渣总黄酮工艺条件优化

采用单因素试验及均匀设计法试验和SPSS 13.0统计软件回归分析,进行微波辅助和超声波辅助提取赣南脐橙皮渣中总黄酮的工艺研究。结果表明：微波辅助最佳提取条件为功率390W、辐射时间7min、乙醇体积分数50%、料液比1:45(g/mL),总黄酮提取可达19.3mg/g;超声波最佳提取条件为温度70℃、超声提取时间60min、乙醇体积分数50%、料液比1:45(g/mL),总黄酮提取可达16.6mg/g。     

响应面优化微波辅助乙醇提取蜂胶黄酮工艺优化

对蜂胶中黄酮类化合物提取工艺条件进行优化。采用单因素试验分析微波时间、微波功率、乙醇体积分数、浸提温度、浸提时间、液料比6个因素对总黄酮得率影响,根据中心组合试验设计原理,采用四因素三水平响应面分析法进行响应面试验,并对各个因素的显著性和交互作用进行分析。结果表明,最优工艺条件为微波时间70s、微波功率282W、乙醇体积分数80%、提取温度77℃、浸提时间12h、液料比25:1(mL/g),在此条件下,蜂胶总黄酮得率为25.08%。     

Optimisation of microwave‐assisted extraction of prune (Prunus domestica) antioxidants by response surface methodology

Optimal conditions for microwave‐assisted extraction (MAE) of total phenols (TP), epicatechin gallate and antioxidant activity from prune (Prunus domestica), rejected in transformation process of plum to prune, were determined by response surface methodology. The central composite design was used to study the effects of three independent variables: microwave power, irradiation time and solvent polarity on the TP, epicatechin gallate and antioxidant activity. Epicatechin gallate was identified as a major phenolic compound in prune extract by RP‐HPLC. Microwave power and irradiation time significantly affected all responses (P < 0.01). The highest TP (598.89 mg GAE/100 g prune) was obtained using water as an extraction solvent at 500 W, during 115 s. However, the optimal conditions for epicatechin gallate extraction were ethanol 80%, 435 W and 120 s. MAE is more efficient than conventional extraction method to obtain TP from prune. The experimental values were reasonably close to the predicted values confirming the validity of the predicted models.     

Microwave‐assisted extraction in goji berries: effect on composition and bioactivity,evaluated through conventional and nonconventional methodologies

This study aimed to evaluate the effect of microwave‐assisted extraction (MAE) parameters on the composition and bioactivity of goji (Lycium barbarum) extracts. Extracts were obtained under a central composite design combination of experimental conditions, and characterised through HPLC‐DAD; their bioactive capacity was ascertained for antimicrobial and antioxidant capacity, the later by spectrophotometric [2,2‐azinobis (3‐ ethylbenzothiazoline‐6‐sulfonic acid) diammonium salt‐radical scavenging activity assay – 413–748 mg ascorbic acid equivalents/100 g DW and oxygen radical absorbance capacity – 1901–2292 mg trolox equivalents/100 g DW] and electrochemical (DNA‐based sensor – 3571–6602 mg ascorbic acid/100 g DW) methods. The quantitative profile of phenolic compounds was strongly dependent on MAE conditions. Significant correlations were found between the presence of several flavonoids and solvent composition, as well as between phenolic acids with methoxy group and the response to DNA‐based sensor. Results may improve targeted extractions for specific compounds, leading to the achievement of extracts richer in antioxidant capacity, as well as in the tailoring of the biosensor response sensitivity to the composition of the extracts under analysis.     

苦丁茶多酚的提取及抗氧化活性

对苦丁茶中多酚的提取及抗氧化活性进行研究。通过单因素和响应面试验可知,在乙醇体积分数52%、料液比1:24(g/mL)、提取时间62s、微波功率291W条件下可获得最高的提取量115.40mg/g。苦丁茶多酚提取液对DPPH自由基、羟自由基、超氧阴离子自由基的半清除质量浓度以及对脂质过氧化的半抑制质量浓度分别为29.24、34.14、872.3、11.48mg/L。表明苦丁茶多酚具有较强的抗氧化作用。     

The optimization of microwave-assisted extraction of decursin from Angelica gigas Nakai root

Response surface methodology was used to display the characteristics of microwave‐assisted extraction (MAE) of soluble solids and decursin from Angelica gigas Nakai root, thereby allowing MAE conditions to be optimized. These included ethanol concentration, microwave power and extraction time. The maximal solid yield was predicted to be 44.2% under conditions of 44.9% ethanol concentration, 115.6 W microwave power and 5.8 min extraction time. Decursin content of the extract was estimated to be maximal at 2.52% using 97.7% ethanol, 90.2 W microwave power, and 6.1 min extraction time. The estimated optimal MAE conditions (67% ethanol, 100 W and 6 min) to maximize both components were verified by comparing estimated values with experimental values (42.2% soluble solids, 2.2% decursin), which were higher than those (35.8% solids, 2.0% decursin) obtained by conventional reflux extraction (60% ethanol, 95 °C and 6 h).     

超声-微波协同提取杜仲树皮及树叶中的黄酮类化合物

为优化杜仲黄酮得率,通过脱胶预处理的杜仲树皮及杜仲树叶为材料,运用超声-微波协同提取方法(UMAE),由单因素实验及响应面法考察UMAE提取工艺条件,并利用HPLC结合标准品比对法比较了树皮与树叶黄酮类成分。结果显示:UMAE的最佳提取条件为乙醇浓度58%,液料比70:1(mL:g),温度75℃,微波功率420 W,时间6 min,此时粗黄酮得率为11.80%±0.09%。将超声-微波协同提取方法与单独微波或单独超声法进行比较,其黄酮得率及抗氧化能力(以清除DPPH自由基能力计)均显著高于单独法(p<0.001)。扫描电镜结果显示,超声波与微波协同作用时,植物细胞壁破碎更为彻底,利于黄酮溶出,因此UMAE提取黄酮的提取效率显著优于单独超声及单独微波的提取方法。通过比较树皮与树叶中黄酮成分的含量,发现杜仲树叶中芦丁、槲皮素、山奈酚含量明显高于树皮,说明杜仲树叶更适用于提取黄酮。     

枣核总黄酮的微波辅助提取工艺优化

目的：采用正交试验法,优选枣核中总黄酮的微波辅助提取工艺。方法：以芦丁为对照品,采用分光光度法进行测定,以枣核黄酮提取率作为考查指标,对影响黄酮提取工艺的因素进行研究。通过单因素试验研究微波功率、提取时间、提取温度、料液比和提取溶剂乙醇体积分数对提取效果的影响。然后,利用正交试验法优化最佳提取工艺条件。结果：对枣核黄酮提取的影响程度大小顺序为料液比＞提取温度＞提取时间＞乙醇体积分数＞微波功率,正交试验结果表明最佳提取工艺参数为料液比1:60(g/mL)、提取温度60℃、乙醇体积分数50%、提取时间20min、微波功率500W。在最佳工艺条件下,枣核黄酮粗品的提取产率为10.14%,粗品中黄酮含量为7.00%。结论：采用正交试验-微波提取工艺,能显著提高枣核黄酮的提取效率,具有较好的提取效果。     

Optimized microwave-assisted extraction of total phenolics (TP) from Ipomoea batatas leaves and its antioxidant activity

An efficient microwave-assisted extraction (MAE) technique was employed to extract total phenolics (TP) from sweetpotato [Ipomoea batatas (L.) Lam.] leaves (TPSL). The optimal conditions for microwave-assisted extraction of TPSL were determined by response surface methodology. A face-centered cubic design (FCD) was applied to evaluate the effects of three independent variables (microwave power, extraction time and ethanol proportion) on the recovery of TPSL. The correlation analysis of the mathematical-regression model indicated that quadratic polynomial model could be employed to optimize the microwave extraction of TPSL. From response surface plots, microwave power, extraction time and ethanol proportion exhibited independent and interactive effects on the extraction of TPSL. The optimal conditions to obtain the highest recovery of TPSL were as follows: microwave power, 302 W; extraction time, 123 s; ethanol proportion, 53% (v/v). Under these optimal conditions, the experimental values agreed with the predicted ones by analysis of variance. It indicated high fitness of the model used and the success of response surface methodology for optimizing TPSL extraction. After method development, the antioxidant activity of the MAE extract was preliminarily evaluated. MAE showed obvious advantages in terms of high extraction efficiency and antioxidant activity of extract with in shortest extraction time.Industrial Relevance: Sweet potato leaves have been neglected except for a partial use as livestock feed in China. This study describes the response surface optimization of microwave-assisted extraction (MAE) process for the enhanced recovery of total phenolics from sweetpotato leaves (TPSL). MAE showed obvious advantages in terms of high extraction efficiency and antioxidant activity of extract within shortest extraction time. TPSL obtained using MAE showed potential for use in health-care food and pharmaceutical industry.     

黑木耳中多酚化合物微波提取工艺

采用L9(34)的正交试验设计,系统研究微波提取黑木耳多酚化合物的工艺条件。以微波功率、微波作用时间、料液比和乙醇体积分数为主要考虑因素,确定了黑木耳多酚化合物微波提取的最佳提取条件为微波作用功率450W、微波作用时间120s、料液比1:25、浸提剂乙醇体积分数75%,此条件下的提取率为0.72%。     

两种微波装置提取柑橘皮总黄酮的工艺比较

分别利用微波化学反应器(简称微化装置)和微波消解/萃取系统(简称微消装置)提取柑橘皮总黄酮。通过L9(34)正交实验设计,以固液比、乙醇浓度、提取时间、微波功率(微化装置)或提取温度(微消装置)为考察因素,分别优化并比较了2种微波装置的提取工艺。微化装置最佳提取工艺条件为:固液比1:30,70%乙醇作提取剂,于240W下微波提取2.0min,此时总黄酮得率为4.72mg/g;微消装置最佳工艺条件为:固液比1:20,70%乙醇作提取剂,于160℃下微波萃取3.0min,此时总黄酮得率为9.15mg/g,得率约为前者的2倍。分析讨论了微消装置得率较高的原因,分别应用2种微波装置提取3个不同品种的柑橘皮样品。结果表明:微消装置提取柑橘皮总黄酮较常规微波辅助提取法更为有效,可用于高效、快速、简便地提取天然产物有效成分。     

山茱萸籽总黄酮的响应曲面法优化微波辅助提取工艺的研究

目的:利用微波辅助提取技术对山茱萸籽总黄酮的提取工艺进行研究。方法:以芦丁为对照品,采用紫外-分光光度法测定山茱萸籽中总黄酮的含量,以总黄酮含量为考察指标,采用响应曲面优化法(RSM)优化山茱萸籽总黄酮的提取工艺。结果:优化的山茱萸籽总黄酮微波辅助提取工艺参数为:微波功率350W,乙醇体积分数50%,液料比20mL/g,提取时间13min。在此最佳条件下,山茱萸籽总黄酮的一次提取率为6.68%。结论:山茱萸籽含有较高的总黄酮含量,所确定的提取工艺提取率高、速度快、操作简便。     

Microwave‐assisted extraction of secoisolariciresinol diglucoside from flaxseed hull

Microwave‐assisted extraction (MAE) of secoisolariciresinol diglucoside (SDG) from defatted flaxseed hull (DFH) was studied. The effects of pre‐soaking methods and extraction parameters (ethanol concentration (0–100%, v/v), microwave energy input (50–390 W), liquid to solid ratio (5:1 to 40:1, mL g^?1) and irradiation time (10–330 s)) on the SDG yield were investigated. Response surface methodology (RSM) was applied to optimise the MAE conditions as irradiation time 90.5 s, ethanol concentration 40.9% (v/v), liquid to solid ratio 21.9:1 (mL g^?1) and microwave power 130 W. The SDG recovery from DFH with MAE was 11.7 g SECO kg^?1 DFH (on dry‐weight basis), which was significantly higher than that of stirring extraction (10.0 g SECO kg^?1 DFH) and Soxhlet extraction (7.60 g SECO kg^?1 DFH). Compared with stirring extraction and Soxhlet extraction, MAE showed its superiority in improving SDG yield and saving time and energy. Copyright © 2007 Society of Chemical Industry