Valorization of sage (Salvia officinalis L.) by-product for recovery of bioactive compounds by novel extraction techniques

Glavni cilj istraživanja ove doktorske disertacije je bio valorizacija sporednog proizvoda žalfije (Salvia officinalis L.) iz fabrike čaja za dobijanje visoko-vrednih ekstrakata željenih osobina koji bi imali primenu u gotovim proizvodima prehrambene, kozmetičke i farmaceutske industrije. U cilju ekstrakcije polifenolnih jedinjenja su primenjene konvencionalne (maceracija) i savremene (ultrazvučna ekstrakcija, mikrotalasna ekstrakcija i ekstrakcija subkritičnom vodom) ekstrakcione tehnike. U postupaku maceracije je optimizovana koncentracija etanola u ekstragensu, dok je za optimizaciju savremenih ekstrakcionih tehnika primenjen eksperimentalni dizajn i metoda odzivne površine. Prinos polifenola (ukupnih fenola i ukupnih flavonoida) i antioksidativna aktivnost određena različitim in vitro testovima su bili ispitivani odzivi. Za svaki od navedenih ekstrakcionih postupaka je ispitivan uticaj glavnih ekstrakcionih parametara: ultrazvučna ekstrakcija (temperatura, vreme ekstrakcije i snaga ultrazvuka), mikrotalasna ekstrakcija (koncentracija etanola, vreme ekstrakcije i odnos rastvarač-droga) i ekstrakcija subkritičnom vodom (temperatura, vreme ekstrakcije i koncentracija HCl u ekstragensu). Tečni ekstrakti dobijeni ultrazvučnom, mikrotalasnom i subkritičnom ekstrakcijom su pokazali izuzetno visoku antioksidativnu aktivnost određenu „hvatanjem“ DPPH i O2∙- radikala i kapacitetom redukcije Fe3+ jona i imali su znatno veći sadržaj polifenola u odnosu na ekstrakte dobijene maceracijom. U cilju ekstrakcije terpenoidnih jedinjenja su primenjeni postupci Soxhlet ekstrakcije, destilacije vodenom parom i ekstrakcije superkritičnim CO2. Postupak superkritične ekstrakcije je optimizovan metodom odzivne površine i optimalni uslovi ekstrakcije su bili pritisak 290 bar, temperatura 55˚C i protok CO2 od 0,4 kg/h, dok su predviđene i eksperimentalne vrednosti prinosa ekstrakcije bile 8,90 i 8,84%. Hemijskom analizom lipofilnih ekstrakata i etarskog ulja je utvrđeno da su oksidovani monoterpeni (α-tujon i kamfor), oksidovani seskviterpeni (viridiflorol) i polifenolni diterpeni (epirosmanol) dominantna jedinjenja prisutna u ovim uzorcima. Tečni ekstrakti žalfije dobijeni konvencionalnim i savremenim ekstrakcionim tehnikama su spray drying tehnikom osušeni u cilju prevođenja u stabilniju formu suvog ekstrakta. Suvim ekstraktima su određene fizičko-hemijske osobine (hemijski sastav, sadržaj vlage, higroskopnost, moć rehidratacije, WAI i WSI) i biološka aktivnost (antimikrobna i antioksidativna aktivnost) i procenjena je njihova mogućnost primene u prehrambenoj i farmaceutskoj industriji.The main aim of this dissertation was valorization of sage (Salvia officinalis L.) by-product from filter-tea factory for recovery of high-value extracts with desirable properties for application in food, cosmetics and pharmaceutical products. Conventional (maceration) and novel (ultrasound-assisted, microwave-assisted and subcritical water extraction) extraction techniques were applied for polyphenols recovery. Ethanol concentration was optimized in maceration process, while experimental design and response surface methodology were applied for optimization of novel extraction techniques. Polyphenols yield (total phenols and total flavonoids) and antioxidant activity, determined by various in vitro assays, were investigated responses. Influence of main process parameters was determined for each technique: ultrasound-assisted extraction (temperature, extraction time and ultrasonic power), microwave-assisted extraction (ethanol concentration, extraction time and sample-solvent ratio) and subcritical water extraction (temperature, extraction time and HCl concentration in solvent). Liquid extracts obtained by novel extraction technique exhibited higher antioxidant activity determined by scavenging of DPPH and O2∙- radicals and reduction of Fe3+ and also provided higher polyphenols yield comparing to extracts obtained by maceration. Soxhlet extraction, hydrodistillation and supercritical fluid extraction were applied for terpenoids recovery. Supercritical fluid extraction process was optimized by response surface methodology and optimal conditions were pressure of 290 bar, temperature of 55˚C and CO2 flow rate of 0.4 kg/h, while predicted and experimentally obtained values of total extraction yield at these conditions were 8.90 i 8.84%, respectively. According to chemical analysis, the most abundant compounds in lipid extracts and essential oil were oxygenated monoterpenes (α-thujone and camphor), oxygenated sesquiterpenes (viridiflorol) and diterpene polyphenols (epirosmanol). Sage liquid extracts obtained by conventional and novel extraction techniques were spray dried in order to obtain dry extract form. Physico-chemical properties (chemical profile, moisture content, hygroscopicity, rehydratation time, WAI and WSI) and biological activity (antimicrobial and antioxidant activity) were determined in dry extracts and their potential application in food and pharmaceutical formulations was discussed

Valorization of sage (Salvia officinalis L.) by-product for recovery of bioactive compounds by novel extraction techniques

Glavni cilj istraživanja ove doktorske disertacije je bio valorizacija sporednog proizvoda žalfije (Salvia officinalis L.) iz fabrike čaja za dobijanje visoko-vrednih ekstrakata željenih osobina koji bi imali primenu u gotovim proizvodima prehrambene, kozmetičke i farmaceutske industrije. U cilju ekstrakcije polifenolnih jedinjenja su primenjene konvencionalne (maceracija) i savremene (ultrazvučna ekstrakcija, mikrotalasna ekstrakcija i ekstrakcija subkritičnom vodom) ekstrakcione tehnike. U postupaku maceracije je optimizovana koncentracija etanola u ekstragensu, dok je za optimizaciju savremenih ekstrakcionih tehnika primenjen eksperimentalni dizajn i metoda odzivne površine. Prinos polifenola (ukupnih fenola i ukupnih flavonoida) i antioksidativna aktivnost određena različitim in vitro testovima su bili ispitivani odzivi. Za svaki od navedenih ekstrakcionih postupaka je ispitivan uticaj glavnih ekstrakcionih parametara: ultrazvučna ekstrakcija (temperatura, vreme ekstrakcije i snaga ultrazvuka), mikrotalasna ekstrakcija (koncentracija etanola, vreme ekstrakcije i odnos rastvarač-droga) i ekstrakcija subkritičnom vodom (temperatura, vreme ekstrakcije i koncentracija HCl u ekstragensu). Tečni ekstrakti dobijeni ultrazvučnom, mikrotalasnom i subkritičnom ekstrakcijom su pokazali izuzetno visoku antioksidativnu aktivnost određenu „hvatanjem“ DPPH i O2∙- radikala i kapacitetom redukcije Fe3+ jona i imali su znatno veći sadržaj polifenola u odnosu na ekstrakte dobijene maceracijom. U cilju ekstrakcije terpenoidnih jedinjenja su primenjeni postupci Soxhlet ekstrakcije, destilacije vodenom parom i ekstrakcije superkritičnim CO2. Postupak superkritične ekstrakcije je optimizovan metodom odzivne površine i optimalni uslovi ekstrakcije su bili pritisak 290 bar, temperatura 55˚C i protok CO2 od 0,4 kg/h, dok su predviđene i eksperimentalne vrednosti prinosa ekstrakcije bile 8,90 i 8,84%. Hemijskom analizom lipofilnih ekstrakata i etarskog ulja je utvrđeno da su oksidovani monoterpeni (α-tujon i kamfor), oksidovani seskviterpeni (viridiflorol) i polifenolni diterpeni (epirosmanol) dominantna jedinjenja prisutna u ovim uzorcima. Tečni ekstrakti žalfije dobijeni konvencionalnim i savremenim ekstrakcionim tehnikama su spray drying tehnikom osušeni u cilju prevođenja u stabilniju formu suvog ekstrakta. Suvim ekstraktima su određene fizičko-hemijske osobine (hemijski sastav, sadržaj vlage, higroskopnost, moć rehidratacije, WAI i WSI) i biološka aktivnost (antimikrobna i antioksidativna aktivnost) i procenjena je njihova mogućnost primene u prehrambenoj i farmaceutskoj industriji.The main aim of this dissertation was valorization of sage (Salvia officinalis L.) by-product from filter-tea factory for recovery of high-value extracts with desirable properties for application in food, cosmetics and pharmaceutical products. Conventional (maceration) and novel (ultrasound-assisted, microwave-assisted and subcritical water extraction) extraction techniques were applied for polyphenols recovery. Ethanol concentration was optimized in maceration process, while experimental design and response surface methodology were applied for optimization of novel extraction techniques. Polyphenols yield (total phenols and total flavonoids) and antioxidant activity, determined by various in vitro assays, were investigated responses. Influence of main process parameters was determined for each technique: ultrasound-assisted extraction (temperature, extraction time and ultrasonic power), microwave-assisted extraction (ethanol concentration, extraction time and sample-solvent ratio) and subcritical water extraction (temperature, extraction time and HCl concentration in solvent). Liquid extracts obtained by novel extraction technique exhibited higher antioxidant activity determined by scavenging of DPPH and O2∙- radicals and reduction of Fe3+ and also provided higher polyphenols yield comparing to extracts obtained by maceration. Soxhlet extraction, hydrodistillation and supercritical fluid extraction were applied for terpenoids recovery. Supercritical fluid extraction process was optimized by response surface methodology and optimal conditions were pressure of 290 bar, temperature of 55˚C and CO2 flow rate of 0.4 kg/h, while predicted and experimentally obtained values of total extraction yield at these conditions were 8.90 i 8.84%, respectively. According to chemical analysis, the most abundant compounds in lipid extracts and essential oil were oxygenated monoterpenes (α-thujone and camphor), oxygenated sesquiterpenes (viridiflorol) and diterpene polyphenols (epirosmanol). Sage liquid extracts obtained by conventional and novel extraction techniques were spray dried in order to obtain dry extract form. Physico-chemical properties (chemical profile, moisture content, hygroscopicity, rehydratation time, WAI and WSI) and biological activity (antimicrobial and antioxidant activity) were determined in dry extracts and their potential application in food and pharmaceutical formulations was discussed

The influence xanthium strumarium l. extracts on maize yield

In several years lasting period occur great numbers of harmful organisms that cause decrease in crops yield. The most frequently occurring weed species cause great damages in agricultural crops, with potential yield loss of 34% [5]. They compete with the crops for water, space, light and nutrients and are hosts to insects and pathogens [8]. During 2014 allelopathic influence of Xanthium strumarium L. on maize yield (Zea mays L.) was studied in field conditions. Beside water extract from plant dry weight of the studied weed species, extract of methanol was also used in different concentrations. Concentrations of 0.04, 0.02, 0.01 and 0.004 g of the plant dry weight per 1 ml of solution were used. The required material was made from weed species picked up in 3-4 leaves phenophases. The reduced maize yield was established in fields in which water extracts, as well as methanol extracts were used. In comparison to untreated control variants, the reduced yield of 10.53-30.3% was established in treatments in which water extracts were applied. In relation to control plots, methanol treatments reduced yield for 20.26-36.32%

Allelopathic effect of Xanthium strumarium L. and Abuthilon theophrasti Med. extracts on germination of maize and soybean seed

During 2014 allelopathic effects of Xanthium strumarium L. and Abutilon theophrasti Med. extracts to germination and initial development of maize (Zea mays L.), and soybean (Glycine max L.) were studied in laboratory conditions. In addition to the Water extracts out of dry mass of the tested weed species, extracts made by use of hexane, ethyl acetate and methanol in different concentrations were also used. The applied concentrations were 10, 20, 30 and 40 g/l of dry matter made out of weed species in the 3-4 leaf stage of development. Inhibiting effect of water extract from dry matter of X. strumarium and methanol extract from which methanol part was evaporated to maize seed epicotyls and hypocotyls length was established. In comparison to the control, the maximum concentration of 40 g / l of the extract made from Water solution of A. theophrasti showed inhibitory effect on soybean seed epicotyls and hypocotyls length. The applied extracts made out of dry matter of the both of the studied weed species X. strumarium and A. theophrasti reduced maize seed germination for 14.8-26.83% and soybean seed germination for 18.5-35.82%, in comparison to the control in which it was 95% and 92%, respectively. After germination in a climate chamber, epicotyls’ and hypocotyls’ length of maize and soybean seeds was measured three, six and ten days following spraying by extracts

Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (Thymus serpyllum L.) Extracts

Funding Information: info:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/UIDB%2F50006%2F2020/PT Funding: This research was supported by the Science Fund of the Republic of Serbia, 6060592, Natural Deep Eutectic Solvents for Green Agri-Food Solutions—DEStiny and 7750168, Novel extracts and bioactive compounds from under-utilized resources for high-value applications—BioUtilize. This project received funding from the European Union’s Horizon 2020—European Research Council (ERC)—under grant agreement No ERC-2016-CoG 725034. T Funding Information: This research was supported by the Science Fund of the Republic of Serbia, 6060592, Natural Deep Eutectic Solvents for Green Agri-Food Solutions?DEStiny and 7750168, Novel extracts and bioactive compounds from under-utilized resources for high-value applications?BioUtilize. This project received funding from the European Union?s Horizon 2020?European Research Council (ERC)?under grant agreement No ERC-2016-CoG 725034. Publisher Copyright: © 2022 by the authors. Licensee MDPI, Basel, Switzerland.Wild thyme (Thymus serpyllum L.) herbal dust has been recognized as a potential underutilized resource for the recovery of antioxidants. The aim of this paper was to optimize natural deep eutectic solvent (NADES) extraction of polyphenols to obtain improved antioxidant activity of extracts determined by selected in vitro assays (DPPH, FRAP, and ABTS). Twenty different NADES systems were investigated in the first step of the screening of the extraction solvent and L-proline (Pro)–glycerine (Gly) based solvents provided the best results. Preliminary experiments organized by 25−1 fractional factorial design narrowed down the number of extraction factors from five (temperature, extraction time, NADES type, water content and L/S ratio) to three and determined their experimental domain for the final step. A face-centered central composite design with temperature (40–55–70 °C), extraction time (60–120–180 min) and L/S ratio (10–20–30 g NADES/g sample) was applied for influence analysis and process optimization. Multi-response optimization suggested a temperature of 65 °C, time of extraction of 180 min and L/S ratio of 28 g NADES/g DW as optimal extraction parameters. Experimental validation confirmed good agreement between experimental and predicted results in the extract obtained at optimal conditions and the interactions in the most suitable NADES (N16; Pro–Gly–H2O; 1:2:1) were confirmed by the1H-NMR.publishersversionpublishe

Isolation of Garlic Bioactives by Pressurized Liquid and Subcritical Water Extraction

Garlic (Allium sativum L.) is widely used in various food products and traditional medicine. Besides unique taste and flavour, it is well known for its chemical profile and bioactive potential. The aim of this study was to apply subcritical water extraction (SWE) and pressurized liquid extraction (PLE) for the extraction of bioactive compounds from the Ranco genotype of garlic. Moreover, PLE process was optimized using response surface methodology (RSM) in order to determine effects and optimize ethanol concentration (45–75%), number of cycles (1–3), extraction time (1–3 min) and temperature (70–110 °C) for maximized total phenols content (TP) and antioxidant activity evaluated by various in vitro assays. Furthermore, temperature effect in SWE process on all responses was evaluated, while allicin content (AC), as a major organosulphur compound, was determined in all samples. Results indicated that PLE provided tremendous advantage over SWE in terms of improved yield and antioxidant activity of garlic extracts. Therefore, high-pressure processes could be used as clean and green procedures for the isolation of garlic bioactives

Simultaneous Hydrolysis of Ellagitannins and Extraction of Ellagic Acid from Defatted Raspberry Seeds Using Natural Deep Eutectic Solvents (NADES)

Grant No. 451-03-9/2021-14/ 200222 Grant no ERC-2016-CoG 72503Defatted raspberry seeds were used as an alternative source of antioxidants and ellagic acid (EA) extracted using Natural deep eutectic solvents (NADES). In the preliminary study, the best NADES combination (citric acid-betaine) and the most influential variables (temperature, time, and NADES/plant ratio) were selected for the further optimization process. All samples were analyzed in terms of total polyphenol, EA content, and antioxidant activity. Two sets of optimal conditions were generated by response surface methodology. The first set (Opt1) was designed for higher conversion of ellagitannins to EA while the latter set (Opt2) for higher EA content/100 g extract. Opt1 and Opt2 had higher values for all investigated responses compared to 80% ethanolic extract but had a lower conversion rate of ellagitannins to EA compared to acidified methanol extract. The third set of parameters (Opt3) selected beyond the initial experimental domain was used to obtain a sample with the highest EA content/100 g extract. Due to their nature, NADES extracts are ready to use and could have various technological roles in products since they are antioxidants, acidifiers, and colorants. NADES raspberry extracts exhibited higher anti-proliferative activity compared to ethanolic extracts in terms of EC50 values. However, the main contributor of anti-cancer activity in NADES raspberry extracts were individual NADES compounds and/or their newly formed NADES structure.publishersversionpublishe

Allelopathic effect of Cannabis sativa L. essential oil on initial growth of Chenopodium album L.

Allelopathy is increasingly gaining importance due to the tendency to avoid the use of synthetic herbicides. Research is increasingly focused on the finding of plant compounds that have allelopathic properties to weed species. The aim the study is to examine the allelopathic potential of Cannabis sativa L. essential oil in relation to the initial growth of the weed species of Chenopodium album L. The essential oil was obtained by the process of distillation of dry plant material collected during the ripening phase. The concentrations of essential oil were 200, 400, 600 and 800ml/l, while distilled water was used in the control. The parameters that were studied were the length of the hypocotyl and the length of the epicotyl C. album L. All investigated concentrations of essential oil exhibited an inhibitory effect. The average length of hypocotyl C. album L. in control was 2.67cm while in the smallest concentration it was 1.9cm. The average length of epicotyl C. album L. in control was 2.7cm and in the lowest applied concentration of 1.67cm. Increasing concentrations of essential oil increased the inhibitory effect. The obtained results indicate that it is possible to use C. sativa L. essential oil as bioherbicides for the control of C. album L