Binary solvent extraction system and extraction time effects on phenolic antioxidants from kenaf seeds (Hibiscus cannabinus L.) extracted by a pulsed ultrasonic-assisted extraction.
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ABSTRACT: The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L.) seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE) were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity assay, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay, β -carotene bleaching inhibition assay, and ferric reducing antioxidant power (FRAP) assay. Total phenolic content (TPC) and total flavonoid content (TFC) evaluations were carried out to determine the phenolic and flavonoid contents in KSE. The KSE from the best extraction parameter was then subjected to high performance liquid chromatography (HPLC) to quantify the phenolic compounds. The optimised extraction condition employed 80% ethanol for 15 min, with the highest values determined for the DPPH, ABTS, and FRAP assay. KSE contained mainly tannic acid (2302.20 mg/100 g extract) and sinapic acid (1198.22 mg/100 g extract), which can be used as alternative antioxidants in the food industry.
Project description:Currently, the analysis of bioactive compounds is easily carried out by modern chromatographic and spectrometric techniques, but the success of the procedure still depends on the efficiency of the extraction methods. This work aimed at finding the optimal conditions for ultrasonic-assisted extraction (UAE) of phenolic antioxidants from grape skin using single-factor experimentation combined with response-surface methodology. Our extraction parameters were ethanol concentration, time and temperature. Total phenolic content (TPC and TPC-280), 2,2-diphenyl-2-picrylhydrazyl (DPPH) radical-scavenging activity and oxygen radical absorbance capacity (ORAC) were dependent variables. A second-order polynomial model satisfactorily described the experimental data. Optimized extraction conditions for UAE from grape skin were: 59.5% ethanol, 113.6 min and 66.8 °C for TPC extraction; 61.1% ethanol, 99.4 min and 66.1 °C for TPC-280 extraction; 57.1% ethanol, 99.5 min and 66.8 °C for DPPH radical-scavenging activity; 60.2% ethanol, 82.4 min and 66.8 °C for ORAC value. Our work provides detailed and useful information to optimize the extraction of grape skin phenols, which are widely used as dietary supplements and nutraceuticals.
Project description:This study evaluates the application of eco-friendly deep eutectic solvents (DESs) in the extraction of phenolic antioxidants from dogbane leaf-tea (DLT). The results showed DESs with lower viscosity allowed an efficient extraction of significantly higher contents of total phenolics or flavonoids. An innovative and high-efficient solvent, choline chloride-levulinic acid (ChCl-LevA), was screened and used in ultrasonic-assisted extraction (UAE) of phenolic compounds from DLT. According to full factorial design experimental results, total phenolic content (TPC), total flavonoid content (TFC), antioxidant activity, and anti-α-glucosidase activity (α-GIA) of the DLT extracts were simultaneously optimized by response surface methodology. Sonication temperature and water content in ChCl-LevA were found to be the major factors affecting the TPC, TFC, antioxidant activity, and α-GIA of DLT extracts. Under the optimum parameters (water content in ChCl-LevA was 45%, sonication temperature was 50 °C, and extraction time was 30 min), the measured results for all the responses were obtained as follows: TPC-91.38 ± 7.20 mg GAE/g DW, TFC-84.12 ± 3.47 mg RE/g DW, ABTS+-492 ± 7.33 mmol TE/g DW, FRAP-6235 ± 121 μmol Fe(II)/g DW and α-GIA-230 ± 7.59 mmol AE/g DW, which were consistent with the predicted values. In addition, strongly significant positive correlations were observed between TPC/TFC and bio-activities of the DLT extracts. HPLC results indicated high contents of (-)-epigallocatechin (4272 ± 84.86 μg/g DW), catechin (5268 ± 24.53 μg/g DW), isoquercitrin (3500 ± 86.07 μg/g DW), kaempferol 3-O-rutinoside (3717 ± 97.71 μg/g DW), and protocatechuic acid (644 ± 1.65 μg/g DW) were observed in the DLT extracts. In contrast to other extraction methods, ChCl-LevA-based UAE yielded higher TPC, TFC, individual phenolic contents, stronger antioxidant activity, and α-GIA. Scanning electron microscope (SEM) analysis further confirmed that ChCl-LevA-based UAE enhanced the disruption of cell wall structure, thereby making more phenolic antioxidants released from DLT. In short, ChCl-LevA-based UAE was confirmed to be an innovative and high-efficient method for extraction of phenolic antioxidants from DLT. Dogbane leaves can be considered as a good tea source rich in natural antioxidants.
Project description:Valorization of onion peel waste, considered to be a rich source of polyphenolic compounds, by employing green extraction techniques is the need of the hour. The aim of the present study was to optimize the microwave-assisted extraction of bioactive phenolic compounds from onion peel wastes employing ChCl:Urea:H2O deep eutectic solvent. Microwave power (100-200-300 W), time (5-15-25 min) and liquid to solid ratio (40:1-50:1-60:1) were studied as the major parameters affecting the extraction efficiency. A Box-Behnken design was adopted including 17 experiments with five centre points. The optimum conditions determined were 100 W microwave power, 15.03 min irradiation time and 54.97 mL g-1 liquid to solid ratio. Under the MAE optimized conditions, the recovery of TPC and FRAP were 80.45 (mg GAE g-1 dw) and 636.18 (µmol AAE g-1 dw), respectively. Morphology of onion peels before and after DES extraction were also studied to gain an insight in the effect of microwave irradiations on the biomass.
Project description:Hawthorn leaves are a rich source of phenolic compounds that possess beneficial activities for human health. Ultrasonic-assisted extraction (UAE) is an extraction technique frequently used for the isolation of phenolic compounds in plants. Thus, in this study, a Box-Behnken design was used to optimize UAE conditions such as the percentage of acetone, the extraction time and solvent-to-solid ratio (v/w) in order to obtain the maximum content of total compounds by Folin-Ciocalteu and the maximum in vitro antioxidant activity by DPPH, ABTS and FRAP assays in Crataegus monogyna leaves. The optimum conditions to obtain the highest total phenolic content and antioxidant activities were 50% acetone, 55 min and 1/1000 (w/v). A total of 30 phenolic compounds were identified and quantified in C. monogyna leaf extract obtained at these optimum UAE conditions. HPLC-MS allows the identification and quantification of 19 phenolic compounds and NP-HPLC-FLD analyses showed the presence of 11 proanthocyanidins. According to the results, the most concentrated phenolic compounds in C. monogyna leaf extract obtained at optimum UAE conditions were phenolic acid derivatives such as protocatechuic acid-glucoside, dihydroxy benzoic acid pentoside and chlorogenic acid, flavones such as 2″-O-rhamnosyl-C-hexosyl-apigenin, flavonols such as hyperoside and isoquercetin and proanthocyanidins such as monomer and dimer. As a result, the optimized UAE conditions could be used to obtain an extract of C. monogyna leaves enriched with phenolic compounds.
Project description:The "ultrasonic-assisted extraction (UAE)" method was utilized in this work to assess how different process parameters affected the yield and recovery of phenolic compounds from the leaf of Commiphora gileadensis, which is one of the medicinal plants with a variety of biological functions. Its leaf is used for a various of therapeutic applications, such as the treatment of bacterial infections, inflammation, and wound healing. The "One-Factor-At-a-Time (OFAT)" approach was employed to examine the impacts of various UAE process parameters on the process of extraction, which include time of extraction, sample/solvent ratio, ultrasonic frequency, and solvent (ethanol) concentration. The extracts were then investigated for the presence of several phytochemicals using analytical techniques such as "Gas Chromatography-Mass Spectroscopy (GC-MS)" and "Fourier Transform Infrared Spectroscopy (FTIR)" studies. The findings showed that the maximum extraction yield, the total phenolic content (TPC), and the total flavonoids content (TFC) of the ethanolic extract of the leaves of C. gileadensis using the UAE method were at 31.80 ± 0.41 %, 96.55 ± 2.81 mg GAE/g d.w. and 31.66 ± 2.01 mg QE/g d.w. accordingly under a procedure duration of 15 min, ultrasonic frequency of 20 kHz, solvent/sample ratio of 1:20 g/mL, and solvent concentration of 40 % v/v. The leaves extract of C. gileadensis included 25 phenolic compounds that were previously unreported, and GC-MS analysis confirmed their presence. Hence, it follows that the UAE technique can successfully extract the phytochemicals from C. gileadensis for a variety of therapeutic uses.
Project description:Polyphenols in carobs have recently attracted great attention due to their wide range of biological and health promoting effects. A comprehensive study was conducted to find an optimum method for the extraction, purification and characterization of these valuable bioactive substances. Under this framework, the ultrasound-assisted extraction (UAE) of polyphenols from carob pulp was optimized by the maximization of the yield in total phenolics using response surface methodology. In particular, the effects of solid-solvent ratio, solvent concentration, extraction time, sonication amplitude, and sonication mode were investigated and optimized using a complete experimental design. In comparison to conventional extraction techniques, UAE offered a higher yield of antioxidants and a shorter processing time. Solid-phase extraction was evaluated as a clean-up strategy prior to the electrophoretic analysis of extracts. The results from the analysis of real samples revealed the predominance of gallic acid and highlighted the great influence of the ripening stage on carobs composition.
Project description:The nutraceutical properties of Punica granatum L. are not restricted to the edible portion of the fruit but also to the peels and seeds, flowers, leaves, and tree bark. The recovery and valorization of the peel and seeds (ca. 50% of the whole fruit), besides the positive environmental impact, can be viewed as a source of natural bioactive compounds. Thus, the bioactive properties of extracts of pomegranate peel and seeds from Acco and Wonderful known cultivars, as well as of the novel Big Full cultivar, were evaluated. The dried and ground pomegranate by-products were submitted to a conventional solid/liquid extraction with ethanol/water mixtures (0%, 25%, 50%, and 75% of EtOH, v/v). The obtained extracts were characterized in terms of total phenolic compounds (TPC), total flavonoids (TF), and antioxidant activity (AA), determined by the DPPH radical scavenging activity and expressed as IC50 (half maximum inhibitory concentration). With the exception of the Acco cultivar, the extraction yield (EY) was higher for peels, whose extracts showed higher TPC, TF, and IC50 (lower AA). The extracts obtained from the by-products of the Big Full cultivar had a statistically higher overall bioactive potential (TPC: 0.36 mg GAE/mg extract; TF: 0.031 mg CATE/mg extract; IC50: 0.51 mg/mL) compared to the other two studied cultivars. Furthermore, the EY was enhanced by solvents richer in ethanol (50-75%), allowing obtaining extracts richer in TPC and TF with higher AA. Finally, it was shown that EY combined with bioactive data allowed a satisfactory principal component unsupervised differentiation of the pomegranate extracts according to the type of by-product used.
Project description:Response surface methodology was used for modeling and optimizing microwave-assisted extraction of antioxidants from Thymbra spicata L. as a factor of temperature, extraction time, solvent concentration, and solvent-to-solid ratio. The prepared extracts showed maximum antioxidant properties, including total phenolic content (TPC), total antioxidant capacity (TAC), and radical scavenging activity (RSA) at the optimum operating conditions. All models calculated for the three responses that are TPC, TAC, and RSA were noteworthy (p < 0.0001) and showed a significant relationship between the response and independent parameters. There was a close relationship between the experimental and the predicted values obtained using the proposed method. The phenolic antioxidant profile of Thymbra spicata L. extract was characterized with the UPLC-PDA-ESI-MS/MS system and rosmarinic acid was found as a major component (1089.2 ± 10.9 mg/100 g-DS). In the future, this optimized and modeled MAE method can be applied in food and pharmaceutical industries to effectively extract antioxidants from edible Thymbra spicata L. plant.
Project description:Extraction solvent is a very important factor in the recovery of antioxidants from natural matrices. In this study, the effect of three solvents (ethanol, ethanol/water and water) on the phenolic composition, antioxidant and anti-cholinesterase activities and electrochemical behaviour of four winemaking byproducts (seeds, skins, stems, and pomace) was evaluated. Phenolic composition was determined by the Folin-Ciocalteu method and ultra-high-performance liquid chromatography (UHPLC), antioxidant activity by the capacity to scavenge 2,2-diphenyl-1-picrylhydrazyl and hydroxyl radicals, anti-cholinesterase activity by the Ellman's method, and electrochemical behaviour by cyclic voltammetry. Eight phenolic compounds were quantified with higher content in water/ethanol extracts (e.g., epicatechin in pomace: 17 mg/100 g vs. 7 and 6 mg/100 g in ethanol and water extracts, respectively), although there were some exceptions (e.g., gallic acid in seeds was most abundant in water extracts). Moreover, the highest total phenolic content (TPC) and antioxidant activity were found in ethanol/water extracts (between 2 and 30-fold the values of the other extracts). Overall, the most active extracts in inhibiting both acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) enzymes were ethanol/water and ethanol extracts from seeds (between 31.11 and 53.90%). The electrochemical behaviour allowed for differentiating the extracts depending on the solvent and the byproduct. Our findings indicate that winemaking byproducts represent a source of phenolic compounds with antioxidant and anti-cholinesterase activities and suggest that cyclic voltammetry is a promising technique to evaluate the phenolic extraction process from these byproducts.
Project description:The ultrasound-assisted extraction (UAE) of oleuropein (OLE), verbascoside (VER), and luteolin-4'-O-glucoside (L4OG), as the major phenolics from olive leaves, was optimized using response surface methodology (RSM). A Box⁻Behnken design (BBD) was used to monitor the effect of different modes of ultrasound operation (pulsed and continuous), liquid⁻solid (L⁻S) ratio, and sonication time on each phenolic yield. The yield of UAE and conventional solid extraction (CSE) was determined after performing ultrahigh-performance liquid chromatography with a diode-array detector (UHPLC-DAD) analysis on the extracts. The results suggested that, under optimal conditions, the concentrations of OLE, VER, and L4OG were 13.386, 0.363, and 0.527 mg/g of dry powdered olive leaves (DPOL), respectively. Verification of experiments was carried out under the modified optimal conditions and the relative errors between the predicted and experimental values were dependent on the examined phenolic compound (OLE 8.63%, VER 11.3%, and L4OG 22.48%). In comparison with CSE, UAE improved the yields of OLE, VER, and L4OG (32.6%, 41.8%, and 47.5%, respectively, after 1 min) at a temperature of 60 °C, an L⁻S ratio of 15 (v/w), and in the continuous mode of UAE. We demonstrated that the UAE technique is an efficient method for enhancing yields of OLE, VER, and L4OG in olive-leaf extracts, while the chosen model was adequate to optimize the extraction of major phenolic compounds from olive leaves.