Ultrasound‐assisted extraction of polyphenols from potato peels: profiling and kinetic modelling

Ultrasound‐assisted extraction (UAE) at 33 and 42 kHz has been investigated in the extraction of polyphenols from peels of two potato varieties, cream‐skinned Lady Claire (LC) and pink‐skinned Lady Rosetta (LR), commonly used in snack food production. Extraction efficacy between the UAE‐untreated (control) and the UAE‐treated extracts was assessed on the total phenolic content and antioxidant capacities (DPPH and FRAP). Application of UAE showed significantly higher recovery of phenolic compounds compared to solid–liquid extraction process alone. Lower ultrasonic frequency (33 kHz) was more effective in recovering polyphenols compared to 42 kHz ultrasonic treatment. The liquid chromatography‐tandem mass spectrometry revealed that chlorogenic acid and caffeic acid were the most prevalent phenolics in LR peels, whereas caffeic acid was dominant in LC peels. Peleg's equation showed a good correlation (R² > 0.92) between the experimental values and the predicted values on the kinetics of UAE of phenolic compounds.     

Characterisation of phenolic extracts from olive pulp and olive pomace by electrospray mass spectrometry

Methanol extracts of olive pomace (two‐phase olive oil extraction) and olive pulp were analysed by reverse phase HPLC and the eluted fractions were characterised by electrospray ionisation mass spectrometry. This technique allowed the identification of some common phenolic compounds, namely, verbascoside, rutin, caffeoyl‐quinic acid, luteolin‐4‐glucoside and 11‐methyl‐oleoside. Hydroxytyrosol‐1′‐β‐glucoside, luteolin‐7‐rutinoside and oleoside were also detected. Moreover, this technique enabled the identification, for the first time in Olea europaea tissues, of two oleoside derivatives, 6′‐β‐glucopyranosyl‐oleoside and 6′‐β‐rhamnopyranosyl‐oleoside, and of 10‐hydroxy‐oleuropein. Also, an oleuropein glucoside that had previously been identified in olive leaves was now detected in olive fruit, both in olive pulp and olive pomace. With the exception of oleoside and oleuropein, the majority of phenolic compounds were found to occur in equivalent amounts in olive pulp and olive pomace. Oleoside was the main phenolic compound in olive pulp (31.6 mg g^?1) but was reduced to 3.6 mg g^?1 in olive pomace, and oleuropein (2.7 mg g^?1 in the pulp) almost disappeared (<0.1 mg g^?1 in the pomace). Both these phenolic compounds were degraded during the olive oil extraction process. Copyright © 2004 Society of Chemical Industry     

Kinetics of ultrasonic extraction of polyphenols,anthocyanins and tannins from five different New Zealand grape pomaces

Polyphenols were extracted from five kinds of New Zealand grape pomace (Sauvignon Blanc, Pinot Gris, Gerwurztraminer, Merlot and Pinot Noir) at 30, 50 and 70 °C in an ultrasonic generator. The extraction kinetics for total phenol, anthocyanin and tannin were determined. The results of dynamics study showed that the extraction of total polyphenols, anthocyanin and tannin followed first-order reaction kinetics during the extraction at 30, 50 and 70 °C. The total phenolic content, anthocyanin conten, and tannin content of water–ethanol extracts from grape pomaces were compared, and the parameters in the extraction kinetics equations were determined. The extraction results showed that the Pinot Noir pomace extract had the highest total phenolic content of 59.95 mg GAE g⁻¹ pomace and tannin content of 79.93 mg EE g⁻¹ pomace. The anthocyanin content in Merlot pomace extract was the highest, which was 4.50 CE g⁻¹ pomace. The results might be of great significance for the development of grape pomace or its polyphenol and/or anthocyanin components as an antioxidant source with natural and inexpensive benefits.     

Determination of antioxidant activity and phenolic compounds of Muntingia calabura Linn. peel by HPLC‐DAD and UPLC‐ESI‐MS/MS

Antioxidant activity in Muntingia calabura Linn. peel was evaluated by DPPH radical, ORAC, ABTS cation radical, FRAP assays and total phenolic contents by different extraction conditions. In addition, a method for determination of phenolic compounds in calabura peel samples harvested in Brazil using methanol:water and magnetic stirring as the extraction method, HPLC‐DAD and UPLC‐ESI‐MS/MS analysis were developed. Calabura peel showed antioxidant activity for all extraction conditions and assays evaluated, the most polar solvents being more effective. The developed HPLC‐DAD method allowed the accurate determination of phenolic compounds, with recoveries in the range of 72–107% and precision values ≤4%, with exception for chlorogenic acid. Gallic acid was determined at the highest concentration levels, followed by myricetin, ferulic acid and vanillic acid. However, all the five proposed phenolic compounds were identified in calabura peel samples by UPLC‐ESI‐MS/MS. Thus, calabura peel, an uncommon edible fruit part, can be appointed as a rich source of phenolic compounds.     

Optimization of a process for enzyme-assisted pigment extraction from grape (<Emphasis Type="Italic">Vitis vinifera</Emphasis> L.) pomace

A process for enzyme-assisted extraction of polyphenols from grape pomace was developed on laboratory and pilot-plant scale. After resuspending grape pomace in water, the skins were ground and the resulting mash was pasteurized to inactivate the deteriorative enzymes responsible for polyphenol degradation, and then pre-extracted with hot water. Subsequently, cell wall polysaccharides were hydrolyzed. The extract was separated from the solid residue by pressing, and finally spray dried. Before scaling-up, enzymatic hydrolysis was optimized on laboratory scale using a D-optimal design and analyzed by response surface methodology. A mixture of pectinolytic and cellulolytic enzyme preparations (ratio 2:1) yielded the highest amounts of phenolic compounds after 2 h of treatment, applying a dosage of 4,500 mg/kg (based on dry matter) at T = 40 °C and pH 4.0. Aqueous pre-extraction of the pomace followed by enzymatic treatment resulted in significantly improved extraction yields reaching 91.9, 92.4, and 63.6% for phenolic acids, non-anthocyanin flavonoids and anthocyanins, respectively. As the yields obtained were comparable to those from sulfite-assisted extraction, this process can be considered a suitable alternative to the application of sulfite.     

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.     

Effect of pulsed electric fields and high pressure on improved recovery of high-added-value compounds from olive pomace

Olive pomace is considered a solid by-product and a rich source of valuable compounds such as polyphenols, flavonoids with antioxidant properties, and proteins. Nonthermal technologies, which cause alterations to cell permeability, are being explored to assist conventional recovery techniques. The aim of this study was to assess the effect of pulsed electric fields (PEF) and high pressure (HP) on improved recovery yield of the high-added-value compounds or to shorten the extraction time of these compounds. Olive pomace (Tsounati cv) was pretreated with PEF (1.0 to 6.5 kV/cm, 0.9 to 51.1 kJ/kg, and 15 µs pulse width) or HP (200 to 600 MPa and 0 to 40 min). Evaluation of the intracellular compounds extracted via solid–liquid extraction (50% ethanol–water solution) was performed. More intense PEF and HP conditions resulted in a significant increase of the phenolic concentration up to 91.6% and 71.8%, respectively. The increased antioxidant capacity of each extract was correlated to phenolic compound concentration. The protein concentration that was achieved with PEF pretreatment was doubled; however, HP-pretreated extracts reached 88.1% higher yield than untreated for pressures up to 200 MPa. HP and PEF pretreatment decreased extraction completion time t₉₈ (needed time to recover the equal amount of phenolics and proteins of untreated after 60 min of conventional extraction) to 12 min and lower than 1 min, respectively. To conclude, both pretreatments are effective in improving the conventional extraction process for increased yield recovery of high-added-value compounds from olive pomace.     

Optimisation of the microwave‐assisted extraction process for six phenolic compounds in Agaricus blazei murrill

An efficient microwave‐assisted extraction (MAE) technique was employed in the extraction of phenolic compounds from Agaricus blazei murrill, and phenolic compounds were quantified by High‐performance liquid chromatography (HPLC). The MAE procedure was optimised, validated and compared with other conventional extraction techniques. MAE gave the best result because of the highest extraction efficiency within the shortest extraction time. The optimal conditions of MAE were 60% ethanol, ratio of solid/liquid 1:30, temperature 110 °C, irradiation power 500 W and three extraction cycles, each 5 min. This is the first report on combining MAE with HPLC for the extraction and quantification of phenolic compounds in A. blazei murrill. The developed MAE method provided a good alternative for the extraction of phenolic compounds in A. blazei murrill as well as other materials.     

Residues of grape (Vitis vinifera L.) seed oil production as a valuable source of phenolic antioxidants

Phenolic compounds of seven grape seed samples originating from mechanical seed oil extraction were identified and quantified by HPLC–DAD before (intact seeds) and after (press residue) the oil recovery process. Total amounts of all identified compounds ranged from 4.81 (‘Cabernet Mitos’) to 19.12 g/kg (‘Schwarzriesling’) of defatted dry matter (DM; ‘Schwarzriesling’) for integral grape seeds, whereas their content in the press residues ranged from 2.80 (‘Cabernet Mitos’) to 13.76 g/kg of defatted DM (‘Spätburgunder’). This is the first study presenting comprehensive data on the contents of individual phenolic compounds comprising all polyphenolic subclasses of press residues from grape seed oil production also covering the determination of the antioxidant activities of each subclass (Folin–Ciocalteu, FRAP and TEAC assays). Additionally, the effects of different solvents on the yields of phenolic compounds were determined. Maximum yields were obtained using methanol/0.1% HCl (v:v), water [75 °C] and a mixture of ethanol and water [3:1; v:v], respectively, whereas pure ethanol resulted in poor polyphenol extraction. The results of the present study confirm the press residues of grape seed oil production still to be a rich source of polyphenolics with strong antioxidant activity.     

Functional compounds from olive pomace to obtain high‐added value foods – a review

Olive pomace, the solid by‐product from virgin olive oil extraction, constitutes a remarkable source of functional compounds and has been exploited by several authors to formulate high value‐added foods and, consequently, to foster the sustainability of the olive‐oil chain. In this framework, the aim of the present review was to summarize the results on the application of functional compounds from olive pomace in food products. Phenolic‐rich extracts from olive pomace were added to vegetable oils, fish burgers, fermented milk, and in the edible coating of fruit, to take advantage of their antioxidant and antimicrobial effects. Olive pomace was also used directly in the formulation of pasta and baked goods, by exploiting polyunsaturated fatty acids, phenolic compounds, and dietary fiber to obtain high value‐added healthy foods and / or to extend their shelf‐life. With the same scope, olive pomace was also added to animal feeds, providing healthy, improved animal products. Different authors used olive pomace to produce biodegradable materials and / or active packaging able to increase the content of bioactive compounds and the oxidative stability of foods. Overall, the results highlighted, in most cases, the effectiveness of the addition of olive pomace‐derived functional compounds in improving nutritional value, quality, and / or the shelf‐life of foods. However, the direct addition of olive pomace was found to be more challenging, especially due to alterations in the sensory and textural features of food. © 2020 Society of Chemical Industry     

Screening grape seeds recovered from winemaking by‐products as sources of reducing agents and mammalian α‐glucosidase and α‐amylase inhibitors

Grape seeds collected from vinification of various grape varieties were extracted by supercritical CO₂ for oil recovery. The defatted residues thus obtained were considered as a re‐utilisable co‐product and assessed for phenolic content, reducing capacity and inhibitory activities against mammalian α‐amylase and α‐glucosidase enzymes. Supercritical CO₂ treatment led to higher recovery of anthocyanins. Reducing capacity of phenolic extracts reached up to ~2200 mmolFe(II) kg^?1, much higher than that of various natural phenolic sources. The anthocyanin‐rich extracts showed the highest inhibitory effectiveness towards α‐glucosidase (I₅₀ value equal to ~40 μg gallic acid equivalents (GAE)/mL ~ half than acarbose). Inhibitory effectiveness towards α‐amylase activity was similar among grape varieties, with I₅₀ values comparable to that of acarbose and correlated with proanthocyanidin contents. These results could pave the way for an efficient processing of grapes, including cascade processes, namely: winemaking, oil extraction from recovered grape seeds and phenolic extraction from defatted grape seeds as potential cost‐effective nutraceuticals.     

Phenolic content,antioxidant and physico‐chemical properties of Sardinian monofloral honeys

In this study, fifty‐one monofloral Sardinian honeys from ten various floral origins were screened for their phenolic content, antioxidant activity, colour and electrical conductivity. The total phenolic amounts have been evaluated by Folin–Ciocalteu method, whereas quantification of several phenolic compounds (phenolic acids and flavonoids) has been carried out by HPLC‐DAD technique. The richest sample in phenolic compounds resulted strawberry tree honey with about 40 mg GAE/100 g, as well FRAP test and DPPH˙ test confirm that antioxidant activity of strawberry tree honey extract exceed both honey extracts and synthetic antioxidants like BHA and BHT. Among the studied phenolic compounds a total of five phenolic acids (ferulic, syringic, trans‐cinnamic, chlorogenic and p‐hydroxycinnamic) and nine flavonoids (catechin, kaempferol, rutin, quercetin, luteolin, apigenin, galangin, pinocembrin and pinobanksin) were identified. Our results show good correlations between total polyphenol amount and antioxidant activity and between colour and electrical conductivity.     

Polyphenols content and antioxidant activity of Ghure (unripe grape) marc extract: influence of extraction time,temperature and solvent type

The objective of this study was to optimise the temperature (25–50 °C), time (1–24 h) and the solvent ratio (ethanol/water, 0–100%) for the phenolic compounds extraction of Ghure marc (unripe grape) using response surface methodology. The central composite design (CCD) generated satisfactory models for the optimisation of process variables. The results revealed that the ratio (X₃) was the most significant parameter on total phenolic content (TPC) and antioxidant activity [% 2‐diphenyl‐1‐picrylhydrazyl (DPPH)], and there was a significant correlation between TPC and antioxidant activity. The optimal conditions for temperature and time were 44.93 °C and 19.34 h, respectively, and the ratio of ethanol to water was 70.08, which verified with carrying out confirmatory experiments. Under this condition, TPC and %DPPH were 388.79 mg GAE per 100 g and 91.01, respectively. The results of this study revealed that the Ghure marc can be used as a low‐cost source of natural antioxidant in food.     

Effect of vacuum‐drying,hot air‐drying and freeze‐drying on polyphenols and antioxidant capacity of lemon (Citrus limon) pomace aqueous extracts

The aim of this study was to investigate the effect of freeze‐drying, hot air‐drying and vacuum‐drying at 70, 90 and 110 °C, on dried lemon pomace polyphenols and antioxidant capacity. The total phenolic content and antioxidant capacity were higher in lemon pomace dried by hot air or under vacuum than those dried by freeze‐drying and increased as the temperature increased. The highest total flavonoid content was recorded in the pomace dried under vacuum at 70 and 90 °C. Lemon pomace dried by freeze‐drying had the highest neohesperidin content, whereas pomace dried under vacuum at 70 °C had the highest rutin and p‐coumaric acid content. The highest gallic acid content was recorded in the pomace dried by hot air at 110 °C. The results of this study indicate that drying technique should be carefully selected according to the bioactive compounds aimed to be extracted.     

High‐pressure recovery of anthocyanins from grape skin pomace (Vitis vinifera cv. Teran) at moderate temperature

The objective was to evaluate the influences of the high hydrostatic pressure extraction parameters on the recovery of anthocyanins from the grape skin pomace extracts (Vitis vinifera cv. Teran) under moderate temperatures. Studied parameters were: solvents (methanol and ethanol); solvent concentrations (30, 50, and 70%); pressures (300, 400, and 500 MPa); times (3, 6.5, 10 min); and temperatures (22, 26, 30 °C). Predominant anthocyanins in all extracts were malvidins (malvidin‐3‐glucoside as the main compound) representing 55.77% of overall anthocyanin content. The type of solvent did not significantly influence anthocyanin extraction yield, while decreased solvent concentration (increased solvent‐to‐water ratio) significantly improved extraction of anthocyanins. Increase of pressure enhanced extraction yield of the anthocyanins but temperature showed stronger impact on the anthocyanins recovery. This investigation evidenced that the best conditions for HHPE of anthocyanins from grape pomace were extraction time 3.39 min, extraction temperature 29.48 °C, pressure 268.44 MPa and solvent concentration 70%.

Practical applications

Due to increased interest for the use of cheap winery byproducts as a source of expensive polyphenols for functional food production, skins from grape pomace became valuable raw material. Therefore, there is a need to evaluate the influence of HHPE innovative extraction technology on its nutritive value during processing. Optimizing parameters for polyphenolic recovery from grape pomace is directly related with nutritional value and economics of food engineering during industrial processing. Obtained results showed that the HHPE under lower temperatures is suitable for the extraction process of anthocyanins from grape skin pomace, but more research is needed to identify other food‐grade solvents with their corresponding concentrations that are useful for the extraction assisted with high hydrostatic pressure.     

Transfer of phenolic compounds during olive oil extraction in relation to ripening stage of the fruit

The transfer of phenolic compounds of Olea europaea L. cv. Arbequina variety during olive oil extraction in relation to ripening stage was investigated. The parameters of oil extraction by the Abencor system are shown together with mass balances of the products and by products from the olive oil extraction in relation to olive paste. The phenolic compounds in olive paste, pomace, oil and wastewater were identified and measured by HPLC. Throughout the study, the concentrations of simple phenols, secoiridoids and flavonoids were higher in the olive paste and pomace phases than in oil and wastewater phases. High concentrations of 4‐(acetoxyethyl)‐1,2‐dihydroxybenzene (3,4‐DHPEA‐AC) and secoiridoid derivatives such as the dialdehydic form of elenolic acid linked to 3,4‐DHPEA (hydroxytyrosol) or p‐HPEA (tyrosol) (3,4‐DHPEA–EDA, p‐HPEA–EDA, where EDA is elenolic acid dialdehyde) and an isomer of oleuropein aglycone (3,4‐DHPEA–EA, where EA is elenolic acid aldehyde) were found in olive oil, together with lignan compounds. It was observed that 3,4‐DHPEA–EDA was the most abundant polyphenol present in the wastewater phase. This indicates that biotransformation occurred during olive extraction, especially in the crushing and malaxation operations, and reflects the possible chemical changes that lead to the formation of new compounds. Moreover, the distribution of compounds showed their affinities toward different phases. Copyright © 2005 Society of Chemical Industry     

Supercritical CO2 extraction of oleanolic acid from grape pomace

In this work, we investigated the possibility to extract oleanolic acid through supercritical fluid extraction from waste materials such as grape pomace, which can represent a yet unexploited source of highly added‐value products. Preliminary supercritical fluid extractions were performed on dried grape skin samples and compared with solid–liquid extraction. After optimising extraction parameters such as temperature, pressure and extraction time, the ratio between supercritical and solid–liquid extraction yields was approximately 1/5. Supercritical CO₂ extractions were also carried out on dried grape pomace samples. In this case, the ratio between supercritical and solid–liquid extraction yields was increased up to 1/3, thanks to a combination of static and dynamic extraction and the use of ethanol as modifier. This extraction technique proved successful in extracting oleanolic acid from grape pomace samples with extraction yields that were comparable with those obtained with well‐established extraction techniques such as solid–liquid extraction.     

Optimization of Extraction of Bioactive Compounds from Different Types of Grape Pomace Produced at Wineries and Distilleries

Natural extracts obtained from grape pomace are particularly interesting, due to the substantial variety of valuable compounds present with health benefits, specifically phenolic compounds such as anthocyanins, trans‐resveratrol, quercetin, and proanthocyanidins. The production of such extracts has been recognized as a profitable way to valorize grape byproducts, which are low‐value and most abundant. First, the effect of the solvent on the extraction of bioactive compounds from grape pomace is studied. The selected solvents are water and ethanol, biocompatible and available in wineries and distilleries. Then, different types of grape pomace obtained along the various stages of current industrial winemaking and distillation processes are analyzed. As a result, the best stage of the winemaking and distillation processes for pomace valorization is identified, corresponding to the grape byproduct with the highest potential as source of bioactive compounds. These studies were performed with Vitis vinifera variety of Tempranillo grapes (same year, same vineyard).     

High‐pressure high‐temperature extraction of phenolic compounds from grape skins

This study focused on the use of a non‐conventional extraction technology by employing high‐pressure high‐temperature stirred reactor to extract polyphenols from grape skins. Extraction time (15–330 min) and temperature (30–150 °C) were selected as independent variables, and their effects were studied. A preliminary kinetic study on polyphenols extraction revealed that the second‐order model fitted satisfactorily the experimental results (R² ≥ 0.9798). Total polyphenol yield and total flavonoid (TF) yield, as well as the antiradical power (ARP) of the extracts, were analysed. The use of high‐pressure high‐temperature technology resulted in obtaining extracts rich in polyphenols with high ARP. The highest total polyphenol (60.7 mg_GAE ) and TF (15.1 mg_CE ) yields were obtained at 150 °C for 270 min and 150 °C for 15 min, respectively. HPLC was employed to analyse phenolic compounds. Considerable quantities of single phenolic compounds were extracted. The highest yields of gallic acid, 5‐hydroxymethylfurfural, protocatechuic acid, catechin, vanillic acid, syringic acid, cumaric acid, trans‐resveratrol and quercetin (163.2, 20.0, 69.9, 420.0, 20.6, 603.0, 20.1, 42.4 and 117.1 mg per 100 g_DS, respectively) were found. ARP values were found between 8.45 and 52.17 μg_DPPH .     

Effect of commercial enzymatic preparation with pectolytic activities on conventional extraction and ultrasound‐assisted extraction of oil from grape seed (Vitis vinifera L.)

Conventional solvent extraction (CE) and ultrasound‐assisted extraction (UAE) in hexane for oil from untreated and enzyme‐treated grape seeds were investigated and compared. Among the output power tested (50, 100 and 150 W) in UAE on untreated seeds, UAE at 150 W for 30 min with liquid‐to‐solid ratio 8:1 (v/w) gave oil extraction yield comparable to CE (ca. 14% w/w) for 6 h with liquid‐to‐solid ratio 12:1 (v/w). CE and UAE at 150 W did not influence the fatty acid profiles of oil. CE oil was found to be the most oxidised. The enzymatic treatments (2, 4 and 6 g per 100 g seeds of Rapidase^® Expression) prior to CE enhanced by 2.5% of the oil yield. Enzymatic treatments higher than 2 g per 100 g seeds increased relative value of some fatty acids both in CE and UAE. Enzymatic pretreatment from 2 to 4 g per 100 g seeds significantly improved some physicochemical parameters of oil quality when extracted by CE, but not by UAE.