Concentration of biologically active compounds extracted from Sideritis ssp. L. by nanofiltration

In the present study experimental results on the nanofiltration of ethanolic extracts from Sideritis ssp. L. are reported, regarding polyphenols and flavonoids concentration and solvent reuse. Three membranes, resistant to organic solvents, have been used: Starmem™ 240 (polyimide), Duramem™ 300 and Duramem™ 500 (both of them modified polyimide). The dependence of the membrane rejection on its MWCO is presented. The separation of flavonoids from phenols with lower molecular weight is found possible at MWCO > 400 Da. A decrease of the flux is observed at permeate to feed volume ratio of about 0.58, thus indicating the existence of a critical concentration, independent of the feed volume and MWCO of the membranes used. The membrane behaviour during nanofiltration has been characterised by ESEM and ATR-FTIR.Concentrations of active compounds up to 3-4 times higher have been obtained in the retentates. The extracts concentrated by nanofiltration preserve their high antioxidant activity. Further dilution of the retentates displays a logarithmic concentration dependence of the radical scavenging activity. The experiments have proved the possibility for permeate use for extraction instead of ethanol, thus essentially reducing the volume of the solvent.     

Supercritical carbon dioxide extraction of triglycerides from Jatropha curcas L. seeds

This study examines the effects of pressure, temperature and solvent to solid ratio (SSR) on extraction efficiency of triglycerides from powdered Jatropha seeds by using supercritical carbon dioxide extraction. Supercritical extractions were designed for pressures ranging from 250 to 350 bar, temperatures ranging from 313 to 333 K and SSR values ranging from 65:1 to 125:1. All values were selected using response surface methodology in order to determine their effects on the concentration of triglycerides from the extracted oil. Using 3750 g of carbon dioxide over 5 h, a supercritical carbon dioxide extraction (at 350 bar, 333 K and an SSR value of 125:1) yielded 43.51% oil. The concentration and extraction efficiency (i.e. recovery) of triglycerides in the extract reached 657.1 mg/g and 97.62%, respectively. Changes in pressure presented more effective in increasing the recovery of triglycerides, but both temperature and the SSR value are important in obtaining high concentration of triglycerides from the Jatropha seeds that are useful for biodiesel materials.     

Extraction of pomegranate (Punica granatum L.) seed oil using superheated hexane

Superheated hexane extraction (SHHE), Soxhlet extraction and cold pressing method were compared for the extraction of pomegranate seed oil. The extraction efficiencies of different temperatures (80, 100, 120 °C), mean particle sizes (0.25, 0.50 and 1.00 mm), and n-hexane flow rates (0.5, 1.0 and 2.0 mL/min) were investigated. The fatty acids profile of the seed oils were quantitatively determined by GC-FID. The optimum extraction temperature, mean particle size, and flow rate were selected as 80 °C, 0.25 mm, and 1 mL/min, respectively. The SHHE showed a higher extraction efficiency (22.18 wt%) within 2 h than Soxhlet extraction (17.94 wt%) for 24 h and cold pressing (4.29 wt%) for 72 h. The fatty acids profile for SHHE was more similar to that obtained by cold pressing method than Soxhlet extraction.     

Extracts from pitanga (Eugenia uniflora L.) leaves: Influence of extraction process on antioxidant properties and yield of phenolic compounds

Different extraction processes were employed to extract the polyphenolic compounds from pitanga (Eugenia uniflora L.) leaves: a one-step process using water, ethanol or supercritical CO₂ as solvents, and a two-step process using supercritical CO₂ followed by either water or ethanol. The total polyphenolic compounds, total flavonoids and antioxidant activity were determined in all the extracts obtained. The process performance was evaluated with respect to three variables: global extraction yield, concentration and yield of both polyphenols and flavonoids in the extracts. For the one-step extraction, the results showed that the extraction yield increased with solvent polarity. For the two-step process, the results suggested that water was more efficient in extracting the phenolic compounds from E. uniflora when the matrix was previously extracted with scCO₂. With respect to the antioxidant activity, the ethanolic extracts obtained from both processes, using either the DPPH radical scavenging method or the β-carotene bleaching method, presented high antioxidant activities.     

Kinetics of ultrasound assisted extraction of anthocyanins from Aronia melanocarpa (black chokeberry) wastes

Black chokeberry fruits are very rich in antioxidant phenolics. After juice extraction, the wastes of pressed berries (juice production by-products) still contain important amount of phenolic species and namely anthocyanins. Ultrasound assisted extraction (UAE) from such wastes was studied. The influence of extraction time (0–240 min), temperature (20–70 °C), solvent composition (0–50% ethanol in water) and ultrasound power (0–100 W) on anthocyanins and polyphenols yields and on antioxidant capacity of the extracts was studied. High temperature and ethanol content in the solvent improved greatly the extraction yields. Ultrasounds improved mainly the extraction kinetics. Ultrasound effect was higher in the beginning of extraction process and at low temperatures. Suitability of UAE for preparation of antioxidant-rich plant extracts at reduced time and energy was confirmed obtaining high extraction efficiencies and high antioxidant capacities of Aronia extracts. To optimize extraction conditions a kinetic mathematical model, based on Peleg's equation and considering also the rate of anthocyanins thermal degradation, was proposed. The influences of extraction time, temperature, solvent composition and ultrasound power on polyphenols and anthocyanins yields and on antioxidant capacity were considered. The optimal conditions for anthocyanins extraction predicted by this model were experimentally validated.     

Extraction of sage (Salvia officinalis L.) by supercritical CO2: Kinetic data, chemical composition and selectivity of diterpenes

The supercritical carbon dioxide (SFE) extraction of Dalmatian sage (Salvia officinalis L.) was investigated and compared to extraction performed by Soxhlet ethanol-water (70:30) mixture extraction (SE) and hydrodistillation (HD). The supercritical extraction allowed isolation of wide spectrum of phytochemicals, while other applied methods were limited to either volatiles (HD) or high molecular compounds isolation (SE). The kinetics of the supercritical extraction and fractionation within the pressure range of 10-30 MPa at 50 °C were also analyzed as well as the chemical compositions of total extract and partial or differential fractions isolated at different CO₂ consumption. Volatile fraction could be isolated at low pressure and low CO₂ consumption, whereby the pressures between 10 and 15 MPa followed by increased CO₂ consumption were favourable for obtaining desired selectivity of diterpenes which contain compounds with expressed antioxidative characteristics.     

Comparison of different extraction methods for the extraction of major bioactive flavonoid compounds from spearmint (Mentha spicata L.) leaves

Different bioactive flavonoid compounds including catechin, epicatechin, rutin, myricetin, luteolin, apigenin and naringenin were obtained from spearmint (Mentha spicata L.) leaves by using conventional soxhlet extraction (CSE) and supercritical carbon dioxide (SC-CO₂) extraction at different extraction schemes and parameters. The effect of different parameters such as temperature (40, 50 and 60 °C), pressure (100, 200 and 300 bar) and dynamic extraction time (30, 60 and 90 min) on the supercritical carbon dioxide (SC-CO₂) extraction of spearmint flavonoids was investigated using full factorial arrangement in a completely randomized design (CRD). The extracts of spearmint leaves obtained by CSE and optimal SC-CO₂ extraction conditions were further analyzed by high performance liquid chromatography (HPLC) to identify and quantify major bioactive flavonoid compounds profile. Comparable results were obtained by optimum SC-CO₂ extraction condition (60 °C, 200 bar, 60 min) and 70% ethanol soxhlet extraction. As revealed by the results, soxhlet extraction had a higher crude extract yield (257.67 mg/g) comparing to the SC-CO₂ extraction (60.57 mg/g). Supercritical carbon dioxide extract (optimum condition) was found to have more main flavonoid compounds (seven bioactive flavonoids) with high concentration comparing to the 70% ethanol soxhlet extraction (five bioactive flavonoids). Therefore, SC-CO₂ extraction is considered as an alternative process compared to the CSE for obtaining the bioactive flavonoid compounds with high concentration from spearmint leaves.     

Supercritical fluid extraction of wormwood (Artemisia absinthium L.)

The objective of the work was to optimize the extraction of wormwood oil by supercritical fluid extraction (SFE) of growth-controlled plant material. Different extraction conditions, two growth techniques and various crops were tested and the evolution of the extracted oil composition was screened chromatographically. A comparison with conventional techniques such as hydrodistillation (HD) or organic solvent extraction (OSE) was also presented. Particularly, six CO₂ densities ranging from 285.0 kg/m³ to 819.5 kg/m³ were studied in the range of 9.0-18.0 MPa and 40-50 °C. A systematic study was carried out with plant material from 2005, while SFE of 2006, 2008 and aeroponically grown crops was performed for comparative purposes. The effect of ethanol as a modifier of the supercritical fluid extraction was also studied. The major compounds found in the SFE extracts as well as in the HD essential oils were Z-epoxyocimene, chrysanthenol and chrysanthenyl acetate. A model based on mass transfer equations, the Sovová model, was successfully applied to correlate the experimental data.     

Extraction of phenolic fraction from guava seeds (Psidium guajava L.) using supercritical carbon dioxide and co-solvents

In this work the supercritical fluid extraction (SFE) with carbon dioxide (CO₂) and with ethyl acetate (EtAc) and ethanol (EtOH) as co-solvents was applied to obtain the phenolic fraction from guava seeds (Psidium guajava L.). The extraction was explored at various operating conditions, using 10, 20 and 30 MPa and 40, 50 and 60 °C. The use of EtAc and EtOH as co-solvents in SFE was also studied. The supercritical process was compared with traditional techniques such as Soxhlet extraction using EtAc and EtOH as solvents. The quality of the different extracts, obtained using SFE and Soxhlet methods and different solvents, was evaluated through the antioxidant activity, obtained by the collection methods of scavenging DPPH and bleaching of β-carotene, and also through the total phenolic content (TPC) of the samples, by the Folin-Ciocalteu method. The antioxidant potential indicates the use of ethanol as co-solvent as the best modifier in SFE, used in concentration of 10% (w/w) at 50 °C and 30 MPa. The quality of the extracts obtained by SFE with EtOH varied with the operating conditions of temperature and pressure, with higher values obtained at 10 and 20 MPa for TPC results and also antioxidant methods. The process yield of the phenolic fraction was also evaluated for all the extraction procedures studied (SFE and Soxhlet), with results varying from 0.380 to 1.738% (w/w).     

Phenolics extraction from Agave americana (L.) leaves using high-temperature, high-pressure reactor

The Agave americana plant has been largely used in traditional medicine. The setting up of efficient methods for phenolics extraction from A. americana leaves is one of great interest. With the aim of optimizing phenolics extraction from this material, the effects of temperature (from 25 to 150 °C) and extraction time (from 15 to 240 min) were investigated using a high-temperature, high-pressure (PARR) reactor, under either air or nitrogen atmosphere. Total polyphenols and flavonoids were determined, and their antioxidant activity was measured by the DPPH radical method. The use of PARR reactor for phenolics extraction proved to be more efficient compared to the conventional solid-liquid extraction at room temperature. The results of this work demonstrated that an increase in both temperature and extraction time led to a corresponding increase in the amount of phenolic compounds extracted and suggested that, after process optimization, this material could be used as an interesting alternative source of polyphenols.     

马齿苋中抑制马拉色菌活性成分的提取工艺研究

采用超声波辅助提取法提取马齿苋中抑制糠秕马拉色菌的活性成分,通过纸片法测定其抑菌效果,并以抑菌效果为指标,采用单因素试验确定较佳提取工艺。结果表明,当提取温度为60℃,提取时间为50 min,料液比为1∶25(g∶mL),超声功率为210 W时,所得提取物的抑菌效果较佳,抑菌圈直径为(46.68±1.21)mm。通过理化反应对马齿苋提取物中的成分进行初步检识,结果表明马齿苋提取物中存在生物碱类、皂苷类、蛋白质多肽或氨基酸和糖类,可能含有鞣质及酚类、黄酮类和三萜类,不存在有机酸类。     

Phytochemical Characterization of Veronica officinalis L., V. teucrium L. and V. orchidea Crantz from Romania and Their Antioxidant and Antimicrobial Properties

Aerial parts of Veronica species are used in Romanian traditional medicine for the treatment of various conditions like kidney diseases, cough, and catarrh, and are known for their wound-healing properties. In the present study, the phenolic and sterolic content and the antioxidant and antimicrobial activities of three Veronica species (Plantaginaceae), V. officinalis L., V. teucrium L. and V. orchidea Crantz, were studied. The identification and quantification of several phenolic compounds and phytosterols were performed using LC/MS techniques and the main components were p-coumaric acid, ferulic acid, luteoline, hispidulin and β-sitosterol. More than that, hispidulin, eupatorin and eupatilin were detected for the first time in the Veronica genus. Nevertheless, representatives of the Veronica genus were never investigated in terms of their phytosterol content. The antioxidant potential investigated by Trolox equivelents antioxidant capacity (TEAC) and EPR spectroscopy revealed that V. officinalis and V. orchidea extracts presented similar antioxidant capacities, whilst the values registered for V. teucrium extract are lower. Regarding the antimicrobial activity of the investigated species, Staphylococcus aureus, Listeria monocytogenes and Listeria ivanovii were the most sensitive strains with MIC values between 3.9 and 15.62 mg/mL. The results obtained by this study may serve to promote better use of representatives from the genus Veronica as antioxidant and antimicrobial agents.     

Preliminary separation and purification of rutin and quercetin from Euonymus alatus (Thunb.) Siebold extracts by macroporous resins

In this study, the performances of rutin and quercetin from Euonymus alatus (Thunb.) Siebold extracts on five macroporous resins with different physical and chemical properties were investigated. The results of static tests indicated that AB-8 resin was the most appropriate and its adsorption data were well fitted to the Langmuir and Freundlich isotherms. In order to optimize the separation process, different pH values of sample solution, different concentrations and pH values of ethanol solution also have been investigated. Column packed with AB-8 resin was used to perform dynamic adsorption and desorption experiments. After the treatment with AB-8 resin and optimal conditions, the contents of rutin and quercetin in the product were 8.45-fold and 13.14-fold increased with recovery yields of 63.1% and 72.3%, respectively. The results showed that the present method was suitable for large-scale preparation of rutin and quercetin from Euonymus alatus (Thunb.) Siebold or other herbal materials.     

Reactive extraction and in situ esterification of Jatropha curcas L. seeds for the production of biodiesel

Jatropha curcas L. has recently been hailed as the promising feedstock for biodiesel production as it does not compete with food sources. Conventional production of biodiesel from J. curcas L. seeds involve two main processing steps; extraction of oil and subsequent esterification/transesterification to fatty acid methyl esters (FAME). In this study, the feasibility of in situ extraction, esterification and transesterification of J. curcas L. seeds to biodiesel was investigated. It was found that the size of the seed and reaction period effect the yield of FAME and amount of oil extracted significantly. Using seed with size less than 0.355 mm and n-hexane as co-solvent with the following reaction conditions; reaction temperature of 60 °C, reaction period of 24 h, methanol to seed ratio of 7.5 ml/g and 15 wt% of H₂SO₄, the oil extraction efficiency and FAME yield can reached 91.2% and 99.8%, respectively. This single step of reactive extraction process therefore can be a potential route for biodiesel production that reduces processing steps and cost.     

The kinetic and thermodynamic analysis of ultrasound-extraction of minerals from aerial parts of white lady's bedstraw (Galium mollugo L.)

The present paper deals with the extraction of some minerals (potassium, calcium and magnesium) from ground, dried aerial parts of white lady's bedstraw (Galium mollugo L.) using an aqueous ethanol solution (50% by volume) at different temperatures (from 23 to 40 °C) in the presence and absence of ultrasound. The main goal was to establish the kinetics and the thermodynamics of the two extraction processes. A phenomenological model involving simultaneous washing and diffusion was proved for both ultrasound-assisted and silent extraction of the minerals. The minerals extraction both in the presence and the absence of ultrasound is endothermic and irreversible since the enthalpy change and the entropy change are positive in the ranges of extraction temperature applied. The Gibbs free energy change for the extraction of minerals is negative, indicating that the process is feasible and spontaneous. The minerals yield increased by a factor of 1.02–1.06 and 1.14–1.27 in the absence and the presence of ultrasound, respectively for every 10 °C rise in temperature.     

Evaluation of Mesua ferrea L. seed oil modified polyurethane paints

Two types of stoving paints have been prepared from Mesua ferrea L. seed oil (MFLSO) modified poly(urethane ester) (PUE) binder systems. One stoving paint system was prepared from partially butylated melamine formaldehyde (MF) resin modified MFLSO-based PUE (70:30 weight ratio) and other one comprised of bisphenol-A-based epoxy resin modified with MFLSO-based PUE (50:50 weight ratio). Paints made with these two resin systems as binders were evaluated against the standard paint system. The physical properties of the paint systems viz. non-volatile content, specific gravity, viscosity, drying time, flexibility, adhesion, scratch hardness, gloss, etc. and chemical properties such as corrosion resistance, salt spray resistance, UV resistance, etc. were measured as per the standard methods and were compared. Thermal stability and surface morphology of the paints were also studied by using thermogravimetric analysis (TGA) and scanning electron microscopy (SEM), respectively. The performance characteristics of both the test paints were found to be comparable with the corresponding industrial standard paints. Out of the two test paints, the epoxy modified PUE-based stoving paint has been found to be preferred.     

Removal of several metal ions from aqueous solution using powdered stem of Arundo donax L. as a new biosorbent

Arundo donax L., a member of Poaceae, was washed, dried, selected, pulverized, and then used for removal of Cu(II), Cd(II), Ni(II), Pb(II) and Zn(II) from aqueous solution. Series batch experiments were conducted to investigate the effects of contact time, pretreatment, particle size of biomass and solution pH on the biosorption capability of A. donax L. powder. The desorption characteristics and renewability of the biomass were also studied. The applicability of Langmuir and Freundlich isotherms was examined for the experimental data, so did the pseudo-first-order, pseudo-second-order and Elovich kinetic models. Results showed that alkali-treated A. donax L. biomass was more appropriate to be the bio-material for biosorption when compared to acid-treated, washed and virgin A. donax L. Owing to its fast adsorption rate, high uptake capacity and the renewability of facility, stem of A. donax L. treated with NaOH seems to be a promising biosorbent for removal of heavy metals from wastewater.     

Guava (Psidium guajava L.) seed oil obtained with a homemade supercritical fluid extraction system using supercritical CO2 and co-solvent

In this work we designed and built a homemade supercritical fluid extraction (HM-SFE) system, in which pure CO₂ and CO₂ with co-solvents were used. The HM-SFE was made by means of thermal dilatation-contraction (TDC). This HM-SFE system was used for obtaining guava (Psidium guajava L.) seed oil, using supercritical CO₂ adding ethanol as co-solvent (CO₂ SC/EtOH), extractions were performed at 313 K and different pressures (10, 20 and 30 MPa), each one in four stages of 30 min, the extract with higher yield was subjected to transesterification and high-resolution gas chromatography (HRGC) analysis. The highest extraction yield was obtained at 30 MPa (17.30% w/w), this yield was higher than one observed in a previous work using SC-CO₂, and near to the one obtained by Soxhlet extraction (20.2% w/w). HRGC enabled the identification of components of the derivatized extract as methyl esters of palmitic, oleic, linoleic, and stearic fatty acids. The results obtained with HM-SFE system was compared with a commercial SFE system, obtained very similar results. In this work was possible to construct a low cost and simple manner HM-SFE system which was employed for obtaining guava seed oil, using CO₂ SC/EtOH.     

Bioethanol production from corn meal by simultaneous enzymatic saccharification and fermentation with immobilized cells of Saccharomyces cerevisiae var. ellipsoideus

The simultaneous enzymatic saccharification and fermentation (SSF) of corn meal using immobilized cells of Saccharomycescerevisiae var. ellipsoideus yeast in a batch system was studied. The yeast cells were immobilized in Ca-alginate by electrostatic droplet generation method. The process kinetics was assessed and determined and the effect of addition of various yeast activators (mineral salts: ZnSO₄ · 7H₂O and MgSO₄ · 7H₂O, and vitamins: Ca-pantothenate, biotin and myo-inositol) separately or mixed, was investigated. Taking into account high values of process parameters (such as ethanol concentration, ethanol yield, percentage of the theoretical ethanol yield, volumetric productivity and utilized glucose) and significant energy savings the SSF process was found to be superior compared to the SHF process. Further improvement in ethanol production was accomplished with the addition of mineral salts as yeast activators which contributed to the highest increase in ethanol production. In this case, the ethanol concentration of 10.23% (w/w), percentage of the theoretical ethanol yield of 98.08%, the ethanol yield of 0.55 g/g and the volumetric productivity of 2.13 g/l·h were obtained.     

Thermostable and flame retardant Mesua ferrea L. seed oil based non-halogenated epoxy resin/clay nanocomposites

Bio-based polymer nanocomposites have a unique niche of their own in the domain of green technology. A bio-based sulfone epoxy resin (BPSE) has been synthesized from the monoglyceride of Mesua ferrea L. seed oil, bis(4-hydroxyphenyl) sulfone, bisphenol-A and epichlorohydrin. The formation of resin was confirmed by the determination of viscosity, epoxy equivalent, etc. and the structure was elucidated from FTIR and ¹H NMR spectroscopies. This resin was used as the matrix for the preparation of epoxy/clay nanocomposites by ex situ technique using different doses of organo nano-clay (1, 2.5 and 5%, w/w). XRD, TEM, SEM, FTIR and rheological studies confirmed the formation of nanocomposites with partial exfoliated structure of the nano-clay. The study demonstrated that the tensile strength enhanced from 4 to 11.4 MPa, scratch hardness improved by two-fold, gloss value increased by 20 units, adhesive strength improved by two-fold and thermal stability improved by 19 °C on incorporation of 5 wt% of nano-clay with respect to the pristine polymer. The limiting oxygen index value and UL94 test indicated improvement of flame retardancy of the nanocomposites. The results exhibit the potentiality of these bio-based epoxy/clay nanocomposites for multifaceted advanced applications.