Antioksidativni i antimikrobni potencijal polifenolnih ekstrakata kupine - uticaj različitih tehnika ekstrakcije i rastvarača
Blackberries (Rubus sp.) are considered a good source of bioactive compounds, especially polyphenols. The high antioxidant and antimicrobial activity associated with polyphenols offers the possibility of using blackberry extracts in various food applications. This study investigates the potential of blackberry extracts obtained with various solvents and extraction techniques as a source of natural antioxidants and antimicrobial compounds. Ethanol and two natural deep eutectic solvents (NADES) (N1 - choline chloride:glycerol (1:2) and N2 - choline chloride:lactic acid (1:4)) and three different extraction techniques (maceration, ultrasound-assisted extraction, and microwave-assisted extraction) were applied. The extracts were evaluated in terms of total monomeric anthocyanin content, polymeric color, total polyphenol content, and ferric reducing antioxidant power (FRAP). The antimicrobial potential against two Gram-positive and two Gram-negative bacteria, as well as one yeast, was assessed using agar diffusion and broth microdilution methods. The N2 solvent gave a better yield of bioactives than N1 and ethanol, while the microwave-assisted extraction had the most pronounced effect on the extracts' polyphenol content and color. All samples displayed significantly higher antimicrobial activity than the ethanolic extract, with the generally highest efficacy observed against Gram-positive bacteria. Overall, these preliminary results demonstrate the potential of acidic NADES for the extraction and application of blackberry polyphenols. Future steps should include extraction optimization and food application studies.
- Research Article
- 10.26554/sti.2025.10.4.1179-1187
- Oct 1, 2025
- Science and Technology Indonesia
The Lempuyang plant is one of the medicinal plants in Indonesia. One of the plants of the Lempuyang family that has not been widely researched is Lempuyang Gajah Zingiber zerumbet (L.). The commonly used method of extraction of phenolic compounds is maceration with organic solvents. The disadvantages are the amount of organic solvents that must be used and the long extraction time (days). An environmentally friendly solvent that has been successfully developed in the 21st century is eutectic or known as Natural deep eutectic solvent (NADES). In addition, NADES can also be used in conjunction with other extraction methods such as (UAE), and microwave aid (MAE). The results obtained were the synthesis of NADES with HBA (Choline Chloride) and HBD variations (Glucose, Lactic Acid, and Ethylene Glycol) with ratios of 1:1 and 1:2. In the maceration process, variations in time (2, 4, 6 hours) and variations in extraction methods (maceration, UAE and UAE-MAE) are carried out. The best TFC (Total Flavonoid Content) value data was obtained by NADES D (choline chloride: glycerol 1:2) of 697.24 mg QE/g extract through a combined ultrasonic and microwave method (UAE-MAE) while the best TPC (Total Phenolic Content) was NADES C (choline chloride: glycerol 1:1) of 2491.88 mg GA/g extract through a combined ultrasonic and microwave method (UAE-MAE). Meanwhile, the characterization of NADES synthesis to see the interaction of hydrogen bonds through FTIR analysis, and the content of phenolic compounds and flavonoids was carried out through HPLC-DAD.
- Research Article
1
- 10.1016/j.procbio.2023.12.025
- Jan 5, 2024
- Process Biochemistry
A green, rapid and efficient protocol for apigenin extraction from Biophytum poterioides Edgew.
- Research Article
- 10.35219/foodtechnology.2025.1.12
- Mar 28, 2025
- The Annals of the University Dunarea de Jos of Galati. Fascicle VI - Food Technology
Date seeds, often considered agro-industrial waste, are a rich source of bioactive compounds such as polysaccharides, mono-oligosaccharides, phytosterols, carotenoids, and polyphenols, all possessing significant functional properties. This review explores the extraction of these compounds using Natural Deep Eutectic Solvents (NADES), a green, biodegradable, and cost-effective alternative to conventional solvents. The extraction efficiency is enhanced when NADES is combined with advanced techniques such as ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), and heating-stirring-assisted extraction (HSAE). Optimal NADES formulations include choline chloride and lactic acid with UAE for polyphenols catechins, choline chloride and ethylene glycol with UAE for polysaccharides, menthol and eucalyptol with HSAE for phytosterols. Additionally, specific NADES combinations facilitate the extraction of carotenoids using Octanoic acid and L-proline with HSAE under controlled conditions. Extracts obtained using choline chloride and ethylene glycol with MAE exhibit promising applications in functional food systems, including food preservation. Notably, polyphenol-rich extracts have been shown to extend the shelf life of Oreochromis niloticus fillets stored at 4°C for up to 10 days. These findings underscore the potential of NADES-extracted date seed components as sustainable food ingredients, aligning with green chemistry principles and contemporary food technology trends.
- Research Article
16
- 10.1016/j.crgsc.2021.100224
- Jan 1, 2021
- Current Research in Green and Sustainable Chemistry
Comparative phenolic content and antioxidant activity of some medicinal plant extracts prepared by choline chloride based green solvents and methanol
- Research Article
111
- 10.1016/j.foodchem.2022.132633
- Mar 5, 2022
- Food Chemistry
Microwave-assisted extraction of antioxidant compounds from by-products of Turkish hazelnut (Corylus avellana L.) using natural deep eutectic solvents: Modeling, optimization and phenolic characterization
- Research Article
11
- 10.1111/jfpe.14503
- Dec 20, 2023
- Journal of Food Process Engineering
This work aimed to optimize the ultrasonic‐assisted extraction (UAE) and microwave‐assisted extraction (MAE) of phenolics and terpenoids from passion fruit peels using natural deep eutectic solvents (NADES). NADES formulated with choline chloride and polyols with organic acids were used to investigate the solubility of phenolics and flavonoids in the solvent. Among these formulations, those derived from lactic acid‐glycerine (LGLY) and citric acid‐glucose (CGLU) exhibited the highest efficiency in extracting phenolics and terpenoids, respectively, when combined with UAE. Then one‐factor experiments were conducted to examine the influence of the UAE conditions (liquid‐to‐solid ratios [LSR], water content in NADES, ultrasonic power, time, and temperature) and MAE conditions (LSR, water content in NADES, ultrasonic power, and time) on the extraction yield of phenolics and terpenoids. The Box‐Behnken design (BBD) model was employed to optimize the extraction conditions with conditional ranges determined based on the results of the one‐factor experiments. The optimal conditions for the CGLU‐based MAE of terpenoids were 387 W of microwave power, 30% water content, 2.4 min, and 20 mL/g of LSR. The optimized conditions for LGLY‐based MAE of phenolics were 299 W, 18.7%, 1.3 min, and 10 mL/g. Total terpenoid content acquired from NADES‐based UAE was higher than NADES‐based MAE, while total phenolic content obtained at the optimal conditions of NADES‐based UAE and MAE was statistically insignificant. The efficiency of the two extraction ways was compared to selecting the favorable extraction method for acquiring phenolics and flavonoids from passion fruit peels. The research proposed that NADES‐based UAE was a green and effective method for attaining phenolics and terpenoids from passion fruit peel.Practical applicationPassion fruit peels are a by‐product of beverage production, which causes environmental pollution and increases treatment costs in the factory. These peels contain various bioactive compounds which benefit human health. The traditional extraction method shows low efficiency and high energy consumption. Thus, the appropriate extraction method and green solvents are needed to improve the extraction efficiency of bioactive compounds and can be directly applied to food products. Ultrasonic‐assisted extraction (UAE) and microwave‐assisted extraction (MAE) combined with natural deep eutectic solvents can enhance the extraction efficiency of bioactive compounds. However, the detailed conditions of UAE and MAE are necessary to compare the performance of the two methods. In addition to showing the significant superiority of UAE with MAE, the research showed the optimized conditions of the UAE process, which can be applied on the industrial scale to extract bioactive compounds and directly add them to food products.
- Research Article
169
- 10.1016/j.foodchem.2022.133871
- Aug 8, 2022
- Food Chemistry
Green extraction of bioactive compounds from apple pomace by ultrasound assisted natural deep eutectic solvent extraction: Optimisation, comparison and bioactivity
- Research Article
27
- 10.3390/plants11202680
- Oct 12, 2022
- Plants
Bilberry fruits (Vaccinium myrtillus L.) are one of the richest natural sources of anthocyanins and are widely used due to their pharmacological and nutritional properties. To ensure their maximum application potential, it is necessary to overcome the limitations of conventional extraction solvents and techniques. This study aimed to develop a green method for bilberry anthocyanin extraction using natural deep eutectic solvents (NaDES) integrated with ultrasound-assisted extraction (UAE) in order to define extraction conditions that will prevent decomposition of the anthocyanins or the loss of bioactivity. After a screening of ten different NaDES, choline chloride:sorbitol (1:1) was selected as the most effective. Furthermore, the influence analysis and optimization of the NaDES–UAE extraction conditions were carried out employing response surface methodology. The optimal conditions were found to be an extraction time of 37.63 min, a temperature of 48.38 °C, and 34.79% (w/w) water in NaDES. The extraction yields of target compounds under optimized extraction conditions were 0.27 mg/g DW of cyanidin-3-O-glucoside and 2.12 mg CGE/g DW of TAC. The obtained optimized extract showed promising radical scavenging and antimicrobial activity. A stability study with the optimized extract revealed that refrigerated storage at 4 °C in the dark provided the best anthocyanins preservation. Overall, the developed NaDES-UAE method showed promising application potential and can be considered as a high-efficiency green alternative to conventional anthocyanins extraction methods, enabling the preservation of active ingredients and the bioactivity of extracts.
- Research Article
17
- 10.3390/plants11152060
- Aug 6, 2022
- Plants
Habanero pepper leaves and stems (by-products) have been traditionally considered waste; however, bioactive compounds such as polyphenols, vitamin C and carotenoids have been identified that can be used for formulation of nutraceuticals or functional foods. Furthermore, the extraction of these bioactive compounds by using environmentally friendly methods and solvents is desirable. Thus, the aim of this study was to assess the antioxidant capacity, total polyphenol content (TPC), the phenolic profile and vitamin C content in extracts obtained from by-products (stems and leaves) of two varieties (Mayapan and Jaguar) of habanero pepper by ultrasound-assisted extraction (UAE) using natural deep eutectic solvents (NADES). The results showed that NADES leads to extracts with significantly higher TPC, higher concentrations of individual polyphenols (gallic acid, protocatechuic acid, chlorogenic acid, cinnamic acid, coumaric acid), vitamin C and, finally, higher antioxidant capacity (9.55 ± 0.02 eq mg Trolox/g DM) than UAE extraction performed with methanol as the solvent. The association of individual polyphenols with NADES was confirmed by principal component analysis (PCA). Overall, NADES is an innovative and promising “green” extraction technique that can be applied successfully for the extraction of phenolic compounds from habanero pepper by-products.
- Research Article
17
- 10.1080/01496395.2022.2112603
- Aug 20, 2022
- Separation Science and Technology
In this study, an environmentally friendly and efficient method based on natural deep eutectic solvent (NADES) in combination with ultrasound-assisted extraction was used for the recovery of phenolic compounds from apple pomace. Acidic, alkaline, sugar-based and polyol-based NADESs were examined for extraction of total phenolic content from apple pomace under different conditions.NADES type, biomass percentage, extraction temperature, extraction time and water content were the testing parameters. NADES type and water content of the solvent were the most important parameters that affected the extraction yield. The most effective NADESs were sugar-based NADESs, which were followed by acidic NADESs. Up to 9.47 mgGAE/gapple pomacewas recovered from apple pomace with glucose:sucrose:water. The highest total flavonoid content was obtained with choline chloride:urea as 17.30 mgEPE/gapple pomace. On the other hand, NADES composed of choline chloride – lactic acid was found to exhibit a significant antioxidant activity. The novelty of this article is the investigation of acidic, alkaline, sugar-based and polyol-based NADESs in the recovery of phenolic compounds from apple pomace using ultrasound-assisted extraction, for the first time in the literature. The antioxidant activity of extracts were also explained in combination with that of NADESs.
- Research Article
4
- 10.3390/pr12102072
- Sep 25, 2024
- Processes
Citrus fruits are widely consumed worldwide; however, one of their primary uses is juice production, resulting in over 40 million tons of agro-industrial waste. Citrus peel is the main agro-industrial by-product in citrus production. In recent years, secondary metabolites of interest, mainly polyphenols such as hesperidin, have been identified in citrus peels. Currently, green alternatives like natural deep eutectic solvents (NADES) based on choline chloride and glucose (Glu), combined with ultrasound-assisted extraction, are studied to obtain polyphenol-rich extracts with potential health applications. This study aims to evaluate the effect of: (1) molar ratios (MR) of 1:0.5, 1:1 or 1:2 mol/mol of choline chloride (ChCl):glucose (Glu); (2) the percentage of added water (WA: 50, 60 or 70%) to NADES; and (3) different citrus peels of Citrus aurantium (bitter orange), Citrus sinensis (sweet orange), and Citrus limon (lemon) used for extraction, on polyphenol profiles, total polyphenol content (TPC), and antioxidant capacity (Ax) of the extracts. The extracts were analyzed using ultra-performance liquid chromatography (UPLC) and evaluated using the Folin–Ciocalteu method for TPC and DPPH assay for quantifying AC. A factorial experimental design 33 was implemented. The extract obtained with an MR of 1:1 (ChCl:Glu) from Citrus aurantium peel exhibited the highest concentration of hesperidin (2003.37 ± 10.91 mg/100 g dry mass), whereas an MR of 1:2 (ChCl:Glu) exhibited the highest concentration of neohesperidin (1045.94 ± 1.27 mg/100 g dry mass), both using 60% WA. This extract also showed the highest antioxidant capacity, achieving 100% inhibition. On the other hand, the highest concentration of total phenolic content (TPC) (96.23 ± 0.83 mg GAE/100 g dry mass) was obtained using C. aurantium peel with an MR of 1:0.5 (ChCl:Glu) and 60% WA. The extracts also presented high concentrations of rutin and catechin. These findings highlight the potential of revalorizing citrus peels, particularly Citrus aurantium, and their extracts obtained with NADES for possible health applications.
- Research Article
67
- 10.3389/fpls.2022.1072592
- Jan 11, 2023
- Frontiers in Plant Science
Conventional extraction techniques are usually based on highly pollutant and/or flammable organic solvents. Therefore, alternative environmentally friendly extraction methods are of particular interest for the recovery of bioactive compounds for their application as food ingredients and/or nutraceuticals. Natural deep eutectic solvents (NADES) are a green and nontoxic attractive alternative to hydroalcoholic extraction. NADES media primarily depends on the intermolecular interactions (hydrogen bonding) among their components to form a eutectic mixture with a much lower final melting point than its individual components. Examples of natural deep eutectic NADES solvents include aqueous solutions (25%–50% water) of choline chloride, sugars, and polyols. This study aimed to investigate the application of two NADES, namely, betaine:triethylene glycol (Bet : TEG) and choline chloride:1,2-propanediol (Chol : Prop), as sustainable green solvents for the extraction of polyphenols from spent coffee ground (SCG), a by-product of coffee processing. In particular, the extraction yield and selectivity were evaluated and compared with conventional green extractions (hot water and a hydroalcoholic solution). In addition, the effect of NADES on the antioxidant and antimicrobial activity of the extracts was investigated. The main outcomes were as follows: (i) NADES were as effective as other conventional green solvents in the extraction of polyphenols with the added advantage of operating at milder temperature conditions, without flammable solvents and with sustainable and natural compounds; (ii) the antimicrobial activity of the NADES extracts was 10 times higher than that of the ethanolic and aqueous extracts. Given the low toxicity of NADES, they could be used as formulation aid for food ingredients.
- Research Article
76
- 10.3390/antiox9111074
- Nov 1, 2020
- Antioxidants
In this study, the recovery of polyphenols from olive oil mill and winery waste was investigated. The performance of ultrasound assisted extraction (UAE), microwave assisted extraction (MAE), and pressurized liquid extraction (PLE) was assessed using ethanol–water mixtures, which are compatible with food, nutraceutical, and cosmetic applications. The extraction efficiency from olive pomace and lees samples was evaluated in terms of total polyphenol content (TPC), determined by high performance liquid chromatography (HPLC) and Folin–Ciocalteu assay. The effect of solvent composition, temperature, and time was analyzed by response surface methodology. Ethanol:water 50:50 (v/v) was found to be a suitable solvent mixture for both kinds of samples and all three extraction techniques. The performance of the extraction techniques was evaluated, under optimal experimental conditions, with a set of different representative samples of residues from olive oil and wine production. Overall, the best extraction efficiency for olive pomace residues was provided by MAE (ethanol:water 50:50 (v/v), 90 °C, 5 min), and for wine residues by PLE (ethanol:water 50:50 (v/v), 100 °C, 5 min, 1 cycle). However, the results provided by UAE (ethanol:water 50:50 (v/v), 30 min) were also suitable. Considering not only extraction performance, but also investment and operational costs, UAE is proposed for a future scaling up evaluation. Regarding olive pomace as a source for natural phenolic antioxidants, olive variety and climatic conditions should be taken into account, since both influence TPC in the extracts, while for winery residues, lees from red wines are more suitable than those from white wines.
- Research Article
8
- 10.1016/j.molliq.2024.125167
- Jun 3, 2024
- Journal of Molecular Liquids
Eco-friendly extraction of six different rosemary (Rosmarinus officinalis L.) genotypes-using natural deep eutectic solvents: Optimization and modeling via response surface methodology (RSM)
- Research Article
7
- 10.22146/ijc.58467
- Jul 26, 2021
- Indonesian Journal of Chemistry
Application of natural deep eutectic solvent (NADES) citric acid-glucose-based microwave-assisted extraction (MAE) method for total polyphenol content (TPC) enriches the use of Eleutherine bulbosa (Mill.) bulb more widely and commercially. Therefore, this study aims to optimize NADES citric acid-glucose-based MAE on the TPC from E. bulbosa bulbs using response surface methodology (RSM). In the present study, the dried sample of E. bulbosa bulb was extracted using the NADES based MAE. Determination of TPC was conducted using Folin-Ciocalteau reagent and standard gallic acid, then measured using a UV-Vis spectrophotometer at 761 nm. Extraction condition optimization of the NADES based MAE method was performed using RSM with Box Behnken Design (four-factors-three-levels and 29 runs) on Design Expert v12. Based on the results study, the optimum condition extraction on the TPC enrichment was obtained at the NADES ratio (citric acid: glucose) 1:1 g/g; solid-liquid ratio 1:8 g/mL; extraction time of 15 min; and 270 Watt microwave power. The confirmation test and scale-up (50 g samples) were obtained with a 61.63 ± 2.23 mg GA/g sample.
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