Influence of ethanol/water ratio in ultrasound and high‐pressure/high‐temperature phenolic compound extraction from agri‐food waste

The valorisation and management of agri‐food waste are currently hot investigation topics which probe the recovery of valuable compounds, such as polyphenols. In this study, high‐pressure/high‐temperature extraction (HPTE) and ultrasound‐assisted extraction (UAE) have been used to study the recovery of phenolic compounds from grape marc and olive pomace in hydroalcoholic solutions. The main phenolic compounds in both extracts were identified by HPLC‐DAD. Besides extraction yield (total polyphenol and flavonoid content) and the antiradical power, polyphenol degradation under HPTE and UAE has also been studied. HPTE with ethanol 75% gave higher phenolic extraction yields: 73.8 ± 1.4 mg of gallic acid equivalents per gram of dried matter and 60.0 mg of caffeic acid equivalents per gram of dried matter for grape marc and olive pomace, respectively. In this study, the efficient combination of ethanol/water mixture with HPTE or UAE has been used to enhance the recovery of phenolic compounds from grape marc and olive pomace. HPLC‐DAD showed that UAE prevents phenolic species degradation damage because of its milder operative conditions.     

Ultrasound-assisted extraction of polyphenols (flavanone glycosides) from orange (Citrus sinensis L.) peel

The present study reports on the extraction of polyphenols especially flavanones from orange (Citrus sinensis L.) peel by using ethanol as a food grade solvent. After a preliminary study showing that the best yield of extraction was reached for a particle size of 2 cm², a response surface methodology (RSM) was launched to investigate the influence of process variables on the ultrasound-assisted extraction (UAE) followed by a central composite design (CCD) approach. The statistical analysis revealed that the optimised conditions were a temperature of 40 °C, a sonication power of 150 W and a 4:1 (v/v) ethanol:water ratio. The high total phenolic content (275.8 mg of gallic acid equivalent/100 g FW), flavanone concentrations (70.3 mg of naringin and 205.2 mg of hesperidin/100 g FW) and extraction yield (10.9 %) obtained from optimised UAE proved its efficiency when compared with the conventional method. Furthermore, the antioxidant activity determined by the DPPH and ORAC tests confirmed the suitability of UAE for the preparation of antioxidant-rich plant extracts.     

Solid-state fermentation of apple pomace using Phanerocheate chrysosporium – Liberation and extraction of phenolic antioxidants

Apple pomace is a by-product from the apple processing industry and can be used for the production of value-added phenolic compounds. A study was carried out to understand the changes and liberation of phenolic compounds and improvement in antioxidant activity during solid-state fermentation of apple pomace using Phanerocheate chrysosporium. The solid-state fermentation of apple pomace using P. chrysosporium mobilised the polyphenolic compounds and improved the nutraceutical properties. The polyphenol content in acetone extract increased and the results were statistically significant (P < 0.05) from 4.6 to 16.12 mg GAE/g dry weight during solid-state fermentation. The effect of various solvents, temperature, time and detergents were also investigated for the extraction of polyphenolics by ultrasonication and microwave-assisted extraction methods. The polyphenol content of the extracts was found to be in the range of 5.78–16.12 mg GAE/g DW of samples, depending on the solvent, extraction time and temperature. Antioxidant activities of polyphenol extracts were tested using the 2,2-diphenyl-1-picryhydrazyl (DPPH) radical methods, where the IC₅₀ ranged from 12.24 to 23.42 μg DW sample, depending on the extraction conditions and the antioxidant activities correlated well with the polyphenol concentrations.     

Chicoric acid from Syringodium filiforme

Detrital and living leaves of the tropical seagrass Syringodium filiforme Kütz. were screened for their phenolic contents. For the first time, the major polyphenols were identified, as chicoric acid (CA) and caftaric acid (CAF), by means of NMR and LC/MS. They were quantified in methanolic and aqueous crude extracts using HPLC. Highest amounts were obtained for extracts sequentially prepared under reflux of methanol, then aqueous-methanol. The concentrations found, respectively, ranged from 0.51 to 1.68 mg (g dw⁻¹) for CAF and 0.94–5.26 mg (g dw⁻¹) for CA (of plant dry mass g dw)⁻¹. This is the first report of CAF in a seagrass and CA in S. filiforme. Considering the demonstrated therapeutic applications of CA, its high value-added on the nutraceutical market, and its rare occurrence in the plant kingdom, the significant content found in S. filiforme leaves makes this abundant renewable raw material of interest for the pharmaceutical and food industries.     

Spray-dried rosemary extracts: Physicochemical and antioxidant properties

In this work, spray-dried rosemary extracts were obtained. A 3³ Box-Behnken design was followed to evaluate the influence of drying conditions on the contents of chemical markers and “in vitro” antioxidant activity of the powder. Although the dry products lost some of their polyphenols, they still had antioxidant activities (IC₅₀) ranging from 17.6 to 24.8 μg · mL⁻¹. Analysis of variance proved that studied factors and some of their interactions significantly affected most of the quality indicators. The best combination of conditions to use for obtaining dry rosemary extracts with adequate physicochemical and functional properties involves an extract feed rate of 6 mL · min⁻¹, a drying air inlet temperature of 140 °C and a spray nozzle air flow rate of 50 L · min⁻¹.     

Antioxidant and antibacterial activities of Nephelium lappaceum L. extracts

Ether, methanolic and aqueous extracts of lyophilized rambutan (Nephelium lappaceum L.) peels and seeds were evaluated for phenolic contents, antioxidant and antibacterial activities. High amounts of phenolic compounds were found in the peel extracts and the highest content was in the methanolic fraction (542.2 mg/g dry extract). Several potential antioxidant activities, including reducing power, β-carotene bleaching, linoleic peroxidation and free radical scavenging activity, were evaluated. The peel extracts exhibited higher antioxidant activity than the seed extracts in all methods determined (P < 0.05). The methanolic fraction was found to be the most active antioxidant as shown by their 50% DPPH inhibition concentration, 4.94 μg/mL. The results indicated this fraction exhibited greater DPPH radical scavenging activity than BHT and ascorbic acid (0.32 g dry extract/g BHT or ascorbic acid). Antibacterial activity against eight bacterial strains was assessed by disc diffusion and broth macrodilution methods. All peel extracts exhibited antibacterial activity against five pathogenic bacteria. The most sensitive strain, Staphylococcus epidermidis, was inhibited by the methanolic extract (MIC 2.0 mg/mL).     

Extraction of resveratrol from the pomace of Palomino fino grapes by supercritical carbon dioxide

Resveratrol is a phenolic compound that is present in grapes and has significant benefits for human health. The development of methods to obtain concentrates of this compound is currently a major challenge in the food industry. In the work described here, resveratrol from grape seeds, stems, skin and pomace of the Palomino fino grape variety was extracted by supercritical carbon dioxide extraction. The effect of pressure (100, 400 bar), temperature (35, 55 °C) and the addition of modifier (5% v/v of ethanol) was evaluated to identify optimal resveratrol extraction from this by-product. Extraction yields and concentrations of resveratrol in the extracts were determined. The best results were obtained on working at high pressure and low temperature using 5% v/v ethanol as a co-solvent.     

Antioxidative and anti-inflammatory properties of Citrus sulcata extracts

Citrus sulcata was subjected to ultrasound, high-pressure, and Soxhlet extractions. The antioxidant and anti-inflammatory activities of the extracts were evaluated qualitatively and quantitatively. The antioxidant content of the peel extract was twice that of the fruit extract. The quantitative analysis showed that the narirutin and hesperidin contents in the peel extracts were 8.8 and 7.5 mg/100 g, respectively. These extracts had a total phenolic content of 112.22 ± 2.89 gallic acid equivalent (GAE) mg/100 g, a total flavonoid content of 54.09 ± 1.01 rutin equivalent (RE) mg/100 g, DPPH radical scavenging activity of 46%, and antioxidant activity of 213.25 ± 2.82 μM of Trolox equivalents (TEAC). C. sulcata extracts could prevent hydrogen peroxide (H₂O₂)-induced oxidative stress, reduce expression of the inflammatory markers nuclear Factor kappa B (NFκB) and phosphorylated IκBα (p-IκBα) in A549 human lung carcinoma cells, and inhibit Lipopolysaccharide (LPS)-induced THP-1 monocyte differentiation to an extent of 85%.     

Characterisation,extraction efficiency,stability and antioxidant activity of phytonutrients in Angelica keiskei

Phytonutrients in Angelica keiskei, a dark green leafy vegetable, were characterised and their extraction efficiency by different compositions of water/ethanol as well as stability at different temperatures was determined. A range in the content of lutein (205–265 mg/kg dry wt), trans-β-carotene (103–130 mg/kg dry wt), and total phenols (8.6–9.7 g/kg) was observed amongst Angelica keiskei grown in three different conditions. LC-ESI-MS/MS analysis identified chlorogenic acid, chalcones and the glucosides of luteolin and quercetin as the major phenolic compounds in Angelica keiskei. Only 46% of lutein was extracted by 70% of ethanol and no carotenoid was detected in 40% ethanol and 100% water extracts of Angelica keiskei. Major phytonutrients in Angelica keiskei were stable at −80 °C up to 12 months whilst β-carotene was significantly degraded at room temperature and 4 °C within 2 months and lutein at room temperature within 12 months.     

Influence of air temperature on drying kinetics and antioxidant potential of olive pomace

This work aims to evaluate the influence of olive pomace drying (a solid by-product of the olive oil industry) on both antioxidant potential and drying kinetics. The two main fractions of olive pomace (pits, PI and pulps + peels, P + P) were characterized by image analysis and density measurement. The drying process was analyzed in experiments carried out at different temperatures (from 50 to 150 °C) and mathematically described from the diffusion and Weibull models. The antioxidant potential of the extracts (ethanol–water 80:20 v/v, 22 ± 1 °C, 170 rpm for 24 h) obtained from the dry product was analyzed by measuring the total phenolic content and antioxidant capacity and the main polyphenols were quantified by HPLC–DAD/MS–MS.     

Kinetic modeling of spice extraction from S. aromaticum and C. cassia

A mathematical model was developed for the extracts obtained from Syzygium aromaticum and Cinnamomum cassia with different particle size, solvent–solid ratios on extraction yield. Different particle sizes in the range of 2.8 mm to ?0.5 mm were employed and maximum extraction efficiency was achieved with particles of size ?0.5 mm. Among the solvent–solid ratios (20:1, 30:1, 40:1 and 50:1) ratio of 50:1 showed higher extraction yield. In the extraction kinetics, higher effective diffusivity value of 36.01 × 10⁻¹⁰ m²/s for S. aromaticum and 26.78 × 10⁻¹⁰ m²/s for C. cassia were achieved. Antioxidant values were determined and extracts prepared from ethanol showed higher scavenging activities for S. aromaticum and C. cassia as 78% and 85% respectively. Maximum phenolic content of 1.6 and 12.4 mg GAE/g of sample were achieved for S. aromaticum and C. cassia by hexane and water respectively.     

The optimisation of extraction of antioxidants from potato peel by pressurised liquids

Response Surface Methodology was used to optimise the solid–liquid extraction and Pressurised Liquid Extraction of polyphenols from industrially generated potato peel. Efficiency of extraction was optimised by measuring antioxidant activity, phenol content and the level of caffeic acid. Conditions for optimal antioxidant activity as measured by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) assay were 75% ethanol, 80 °C and 22 min with solid–liquid extraction, resulting in an optimum activity of 352 mg Trolox Equivalents/100 g DW potato peel. In comparison, the use of Pressurised Liquid Extraction resulted in an optimum activity of 339 mg Trolox Equivalents/100 g DW potato peel at 70% ethanol and 125 °C. Therefore the use of Pressurised Liquid Extraction did not enhance extraction in comparison to solid–liquid extracts, but using aqueous ethanol as extraction solvent recovered a higher level of polyphenols than when using 100% methanol.     

Cellulase-assisted release of secoisolariciresinol from extracts of flax (Linum usitatissimum) hulls and whole seeds

Extraction of secoisolariciresinol from seed hulls and whole seeds of flax was improved using an enzymatic step with cellulase R10 from Trichoderma reesei that allowed better yield as compared to β-glucosidase. The cellulase assisted extraction process was further optimised for different parameters such as duration and concentration of hydromethanolic extraction, duration of alkaline hydrolysis, pH, duration and incubation temperature as well as enzyme concentration. Best results were obtained using a method including the following successive steps: 16 h of 70% hydromethanolic extraction, 6 h of 0.1 M sodium hydroxide hydrolysis followed by a 6 h incubation with 1 unit ml⁻¹ of cellulase R10 in 0.1 M citrate–phosphate buffer pH 2.8 at 40 °C. Under these conditions, all forms of the main flax lignan were recovered as the aglycone form, i.e. secoisolariciresinol. Highest yields in secoisolariciresinol diglucoside (SDG) equivalent reached 7.72% of flaxseed hull (cv. Baladin) dry weight and 2.88% of whole seed (cv. Barbara) weight, thus allowing a significant improvement in comparison with published methods.     

Apple pomace as a source of dietary fiber and polyphenols and its effect on the rheological characteristics and cake making

Apple pomace, a by-product of apple juice industry, is a rich source of fibre and polyphenols. Also in view of the antioxidant property of pomace, it would play an important role in prevention of diseases. Apple pomace procured from fruit juice industry, contained 10.8% moisture, 0.5% ash and 51.1% of dietary fibre. Finely ground apple pomace was incorporated in wheat flour at 5%, 10% and 15% levels and studied for rheological characteristics. Water absorption increased significantly from 60.1% to 70.6% with increase in pomace from 0% to 15%. Dough stability decreased and mixing tolerance index increased, indicating weakening of the dough. Resistance to extension values significantly increased from 336 to 742 BU whereas extensibility values decreased from 127 to 51 mm. Amylograph studies showed decrease in peak viscosity and cold paste viscosity from 950 to 730 BU and 1760 to 970 BU respectively. Cakes were prepared from blends of wheat flour containing 0–30% apple pomace. The volume of cakes decreased from 850 to 620 cc with increase in pomace content from 0% to 30%. Cakes prepared from 25% of apple pomace had a dietary fibre content of 14.2% The total phenol content in wheat flour and apple pomace was 1.19 and 7.16 mg/g respectively where as cakes prepared from 0% and 25% apple pomace blends had 2.07 and 3.15 mg/g indicating that apple pomace can serve as a good source of both polyphenols and dietary fibre.     

Determination of isoflavone content and antioxidant activity in Psoralea corylifolia L. callus cultures

Relation between isoflavones production and antioxidant activity in Psoralea corylifolia cell cultures was studied. High performance liquid chromatography analysis revealed that root-derived callus cultures produced maximum amount of daidzein whereas genistein by leaf-derived callus. Cell cultures grown under continuous illumination (40-μmol m⁻² s⁻¹) produced several-fold more isoflavones daidzein (2.28% dry wt) and genistein (0.21% dry wt) than that of field grown plants. The antioxidant activity of extracts was determined using 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay, phosphomolybdenum assay and correlated with the content of total phenolics in the extracts. Calli grown under continuous illumination exhibited strong antioxidant activities compared to dark grown callus cultures and explants materials.     

Changes in bioactive compounds and antioxidant capacity of fresh-cut cashew apple

In this study, ascorbic acid, total polyphenols and proanthocyanidins of fresh-cut cashew apple were quantified. Antioxidant capacity was determined in whole juice and in polyphenols extracts by three methods: 2,2-diphenyl-1-picrylhydrazyl (DPPH), ferric reducing antioxidant power (FRAP) and ??-carotene bleaching. Effect of cutting and storage for 24 h at 2 °C, 27 °C and 40 °C on these compounds were also evaluated. Cashew apple presented 163 mg of ascorbic acid per 100 g of fresh weight (FW). Soluble and hydrolysable polyphenols contents were 12.79 mg GAE/100 g FW and 18.53 mg GAE/100 g FW and proanthocyanidins were 9.27 mg/100 g FW. Antioxidant capacity of juice and polyphenols extract was high for DPPH method. Storage temperatures affected bioactive compounds on cut cashew apple. The content of ascorbic acid decreased in all temperatures. Proanthocyanidins were more sensitive to 40 °C than to other temperatures. The content of polyphenols and antioxidant capacity of juice by DPPH assay did not change. However, the reducing power was lower in samples kept at high temperatures. A strong positive correlation between ascorbic acid and FRAP (r = 0.99) and a negative correlation between DPPH and FRAP (r = − 0.79) were observed. No correlations were found between polyphenols and antioxidant capacity indicating the importance of phenolic composition in the extracts. The results confirm the importance of temperature and injury on the quality of cashew apple.     

Effect of ionising radiation on polyphenolic content and antioxidant potential of parathion-treated sage (Salvia officinalis) leaves

The γ-irradiation effects on polyphenolic content and antioxidant capacity of parathion-pretreated leaves of Salvia officinalis plant were investigated. The analysis of phenolic extracts of sage without parathion showed that irradiation decreased polyphenolic content significantly (p < 0.05) by 30% and 45% at 2 and 4 kGy, respectively, compared to non-irradiated samples. The same trend was observed for the Trolox equivalent antioxidant capacity (TEAC), as assessed by the anionic DPPH and cationic ABTS radical-scavenging assays. The antioxidant potential decreased significantly (p < 0.01) at 2 and 4 kGy, by 11–20% and 40–44%, respectively. The results obtained with a pure chlorogenic acid solution confirmed the degradation of phenols; however, its TEAC was significantly (p < 0.01) increased following irradiation. Degradation products of parathion formed by irradiation seem to protect against a decline of antioxidant capacity and reduce polyphenolic loss. Ionising radiation was found to be useful in breaking down pesticide residues without inducing significant losses in polyphenols.     

Optimisation of microwave-assisted enzymatic extraction of corilagin and geraniin from Geranium sibiricum Linne and evaluation of antioxidant activity

Plant polyphenols exhibit effective bio-activities, particularly antioxidant activities. Previous studies showed that Geranium sibiricum Linne contains high levels of polyphenolic compounds such as corilagin (CG) and geraniin (GE). In this study, a microwave-assisted enzymatic extraction (MAEE) method was evaluated for the simultaneous extraction of CG and GE only with deionised water. The optimal extraction conditions were as follows: irradiation power 500 W, ratio of solvent to material 40 ml/g, irradiation temperature 33 °C, pH 5.2, amount of cellulase 3600 U/g and irradiation time 9 min. Under these conditions, the extraction yields of CG and GE achieved were 6.79 and 19.82 mg/g, which increased by 64.01% and 72.95%, respectively, as compared with the control ones. Furthermore, the antioxidant activities of crude extracts were 2.61 mmol FeSO₄/g DW and 0.118 mg/ml (IC₅₀), according to the FRAP and DPPH assays, which indicated G. sibiricum Linne possesses good potential for natural antioxidants.     

Antioxidant, antiacetylcholinesterase and antimicrobial activities of Cymbopogon schoenanthus L. Spreng (lemon grass) from Tunisia

Aqueous extract, proanthocyanidin rich extract, and organic extracts of Cymbopogon schoenanthus L. Spreng (lemon grass) shoots from three different locations in South Tunisia were screened for their antioxidant, acetylcholinesterase and antimicrobial activities. In addition to the evaluation of these activities, the contents of flavonoids and total phenolic compounds were determined.Antioxidant activity measured by DPPH assay showed that the proanthocyanidin extract exhibited higher antioxidant activity than the aqueous extract. Extract concentration providing 50% inhibition (IC₅₀) ranged from 16.4 ± 6.8 μg/mL to 26.4 ± 6.8 μg/mL. The antioxidant activity was also determined using the β-carotene/linoleic acid bleaching test. The best results (IC₅₀ = 0.11 ± 0.10 mg/mL) were obtained with the proanthocyanidin extract of the plants collected from the desert region (Dhibat).The greatest acetylcholinesterase inhibitory activity (IC₅₀ = 0.23 ± 0.04 mg/mL) was exhibited by the ethyl acetate and methanol extracts of the plants collected from the mountainous region. It seems that extracts obtained with more polar solvents gave better results.The proanthocyanidin extracts showed a good antimicrobial activity against Streptococcus sobrinus at low concentration (MIC = 4 mg/mL). Therefore, these extracts could be used to prevent carious lesions by inhibiting S. sobrinus growth.     

Distribution of caffeic acid derivatives in Gundelia tournefortii L.

The caffeic acid derivatives including neochlorogenic acid (3-COA), cryptochlorogenic acid (4-CQA), chlorogenic acid (5-CQA) and caffeic acid (CA) have been characterised in Gundelia tournefortii using reference compounds, chemical, spectral evidences and chromatographic data. In addition, the total phenolic content and chlorogenic acid were measured in the leaf, hull-less seed, and skin extracts of this herb by the Folin–Ciocalteu reagent and high performance liquid chromatography (HPLC), respectively. The sample analysis was carried out on a C₁₈ column with 5% (v/v) aqueous acetic acid and methanol as the mobile phase, under gradient elution at ambient temperature, at 325 nm. The amount of chlorogenic acid in the leafs (at the flowering stage and after it) and hull-less seed were 984, 466 and 199 mg per 100 g dry plant sample and the total phenolic content in their dry extract were 128.4, 103.8 and 76.3 μg/mg as CGA equivalent, respectively.