Optimisation of supercritical CO2 extraction of grape seed oil using response surface methodology

The aim of this study was to use waste from the wine production process with special accent on grape seeds and new green technology. Supercritical CO₂ was considered as a green solvent in extraction of grape seed oil. The effects of different extraction process parameters on oil yield and antioxidant activity were investigated. Extraction optimisation was conducted using response surface methodology (RSM). Extraction pressure has proven to be the most significant factor influencing oil yield and antioxidant activity (P < 0.0001). The optimal conditions for obtaining the highest oil yield and antioxidant activity within the experimental range of the variables studied were at extraction pressure of 400 bar and temperature of 41 °C. Under these optimal conditions, the predicted extraction oil yield was 14.49% and DPPH 37.07%. Applying this green extraction method, the oil from grape seeds was totally extracted. The produced oil was of satisfactory quality, and the content of α‐tocopherol in obtained grape seed oil at optimal extraction conditions was 36.05 mg kg^?1.     

Preparation,antioxidant activity and protective effect of coconut testa oil extraction on oxidative damage to human serum albumin

Extraction, physicochemical properties and fatty acid composition analysis of coconut testa oil (CTO), antioxidant activity and the protective effect on oxidative damage to human serum albumin (HSA) of coconut testa oil extract (CTOE) were investigated. Results showed that the optimal extract condition of CTO was B₃A₂C₂ (temperature of 60 °C, material‐to‐solvent of 1:4 g mL^?1 and extraction time of 3 h) with the maximum oil yield (76.83 ± 0.53%). The obtained CTO was nondrying oil with iodine value of 14.69 g per 100 g, and lauric acid was the main component of 42.28%. Hydrogen peroxide scavenging activity of CTOE can reach to 49.81% at 2.5 mg mL^?1, while antioxidant activity (AA) on the oxidation of linoleic acid dropped from 56.82% to 31.70% during the first 80 min. CTOE could prevent HSA from oxidative damage induced by hydrogen peroxide via inhibiting the formation of protein carbonyl and increase of hydroperoxides content effectively. Total phenolic content was 68 mg g^?1, and the epicatechin and catechin were 2.74 and 2.26 mg g^?1 in its phenolic compositions, respectively. These all suggested CTO and CTOE might be new worthy exploiting functional sources.     

Composition and biological activities of the essential oil from Schisandra chinensis obtained by solvent-free microwave extraction

Applicability of solvent-free microwave extraction (SFME) for extraction of the fruits of Schisandra chinensis essential oil was examined; the composition and antioxidant activities and antibacterial activities of the essential oil were assessed in vitro. An orthogonal experiment (L₉ (3)⁴) was applied to optimize the extraction process. The optimum conditions were: extraction time, 45 min; microwave power, 800 W; diameter of powder particles, 0.25 mm; and proportion of water pretreatment, 30%. Under these conditions, the extraction yield was 1.75%. Thirty-five compounds, representing 91.12% of the oil, were identified, of which the major ones, ylangene (50.11%), β-himachalene (10.76%)，α-bergamotene (9.52%) and β-Chamigrene (5.41%), accounted for of 75.80% the oil.Antioxidant activity, IC₅₀ value of the essential oil was determined as 3.87 mg/mL by DPPH assay, and the inhibition values of the essential oil at 1.8 mg/mL was 41.88% by β-Carotene–linoleic acid bleaching assay. The essential oil was screened for antibacterial activity against both Gram positive (Staphylococcus epidermidis, Staphylococcus aureus, Bacillus subtilis) and Gram negative (Escherichia coli, Pseudomonas aeruginosa, Proteus vulgaris) bacteria. The essential oil showed antibacterial effect against all the gram (+) bacteria and gram (−) bacteria tested. These results show that S. chinensis essential oil could be considered as a natural alternative to food antioxidants and preservatives.     

Process optimisation of microwave‐assisted extraction of peony (Paeonia suffruticosa Andr.) seed oil using hexane–ethanol mixture and its characterisation

Ethanol and hexane mixture agent microwave‐assisted extraction (MAE) method was conducted to extract peony (Paeonia suffruticosa Andr.) seed oil (PSO). The aim of the study was to optimise the extraction for both yield and energy consumption in mixture agent MAE. The highest oil yield (34.49%) and lowest unit energy consumption (14 125.4 J g^?1) were obtained under optimum extraction condition: solid‐liquid ratio 0.37 g mL^?1, extraction time 3.72 min, extraction temperature 80.92 °C, ethanol ratio 20.00%. GC–MS results showed that unsaturated fatty acids (UFAs) accounted for 88.60% of total fatty acids in PSO. Moreover, linolenic acid content of 37.35% was the highest UFA and caused PSO to possess good nutrition. PSO in DPPH radical scavenging experiment showed that IC₅₀ value of 28.80 ± 2.13 mg mL^?1 exhibited strong antioxidant property. All experiments proved that mixed solvent MAE is an efficient and promising method to extract PSO. This method can effectively reduce the energy consumption and extraction time.     

The antioxidant capacity of polysaccharide from Laminaria japonica by citric acid extraction

An optimal citric acid extraction condition (pH 2.0; extraction temperature: 120 °C; extraction time: 3 h) was developed to obtain polysaccharide from Laminaria japonica. The yield of polysaccharide was 13.31 ± 0.08%, with IC₅₀ value of DPPH radical scavenging activity of 0.98 ± 0.01 mg mL^?1. The viscosity of polysaccharide extracted by citric acid (LJPA) was eight times lower than that of polysaccharide extracted by hot water (LJPW), which may be attributed to the low average molecular weight of LJPA (17.12 kDa). Gas chromatography analysis indicated that LJPA was composed of rhamnose, fucose, xylose, manose, glucose and galactose with relative molar percentages of 4.51%, 20.27%, 12.43%, 12.81%, 10.29% and 39.69% respectively. Furthermore, LJPA exhibited significantly higher antioxidant capacities including oxygen radical absorbance capacity (ORAC), ABTS radical scavenging activity and reducing power than LJPW. Citric acid extraction showed a positive influence on the polysaccharide degradation and antioxidant capacities of L. japonica.     

Mechanochemical‐assisted extraction and antioxidant activity of polysaccharides from Ganoderma lucidum spores

Mechanochemical‐assisted extraction (MCAE) method was developed to an effective method for polysaccharides extraction from Ganoderma lucidum spores. The MCAE parameters and the antioxidant activity of polysaccharides were investigated. Through response surface methodology design experiments, the processing conditions were optimised as follows: material/solid reagent (Na₂CO₃) 5 g·g^?1, milling time 20 min, solution/material ratio twenty (mL·g^?1) and extraction time 130 min. Under these conditions, the yield of polysaccharides was (5.92 ± 0.13)%, which was in close agreement with the predicted value. Compared with the heat‐reflux extraction method, the MCAE method had higher extraction yield, shorter extraction time and lower extraction temperature. In addition, the polysaccharides obtained from MCAE exhibit significant antioxidant activity.     

The Phenolic Compounds,Metabolites, and Antioxidant Activity of Propolis Extracted by Ultrasound‐Assisted Method

The influences of ultrasound‐assisted, pharmacopeia, and supercritical fluid extraction methods on bioactive compounds and biological activities of propolis were evaluated. Results showed that propolis extracted by ultrasound‐assisted method contained more phenolic compounds, and showed the highest total phenolic content (245.84 ± 6.41 mg GAE/g DW), total flavonoids content (198.82 ± 5.74 mg RE/g DW), and stronger in vitro antioxidant activity (DPPH·: 1.03 ± 0.04 mmol Trolox/g DW, ABTS+·: 2.19 ± 0.05 mmol Trolox/g DW, and FRAP: 1.48 ± 0.12 mmol FeSO₄/g DW) than those of pharmacopoeia and supercritical fluid methods. A total of 36 phenolic compounds were identified in propolis. Among them, quercetin, quercetin‐3‐methyl‐ether, kaempferol, isorhamnetin, luteolin‐methyl‐ether, and quercetin‐7‐methyl‐ether could only be found in ultrasound‐assisted and pharmacopoeia methods. Moreover, the phenolic compounds had the similar metabolic pathways in rats and were mainly metabolized by sulfation and glucuronidation pathways. Additionally, ultrasonic‐treated propolis have good in vivo antioxidant activity and could repair D‐galactose‐induced oxidative damage in rats. Therefore, ultrasound‐assisted method could replace pharmacopeia method to be considered as bioactive compounds extraction from propolis, taking into consideration of yield, short extraction time, and high antioxidant activity.     

Chemical composition,antioxidant activity and anti‐lipase activity of Origanum vulgare and Lippia turbinata essential oils

This study reported the chemical composition, phenolic content, antioxidant and anti‐lipase activity of oregano and Lippia essential oils. The major compounds found in oregano essential oil were γ‐terpinene (32.10%), α‐terpinene (15.10%), p‐cymene (8.00%) and thymol (8.00%). In Lippia essential oil, α‐limonene (76.80%) and 1,8‐cineole (4.95%) represented the major compounds. Oregano essential oil had higher phenolic content (12.47 mg gallic acid mL^?1) and DPPH scavenging activity (IC₅₀ 0.357 μg mL^?1) than Lippia essential oil (7.94 mg gallic acid mL^?1 and IC₅₀ 0.400 μg mL^?1, respectively). Both essential oils had similar antioxidant indexes (about 1.2) determined by Rancimat. Moreover, oregano essential oil had also higher anti‐lipase activity (IC₅₀ 5.09 and 7.26 μg mL^?1). Higher phenolic content in the essential oils was related with higher scavenging and anti‐lipase activities. Oregano and Lippia essential oils could be used as natural antioxidants on food products.     

Antioxidant peptides isolated from sea cucumber Stichopus Japonicus

The sea cucumber Stichopus japonicus protein was hydrolyzed by pepsin, trypsin, papain, acid protease and neutral protease, respectively, to get five kinds of peptide fractions: pepsin peptides (PP), trypsin peptides (TP), acid protease peptides (AP), neutral protease peptides (NP) and papain peptide (PAP). Antioxidative activities of all peptide fractions were evaluated by hydroxyl radical– (·OH) and Superoxide anion (O₂ ^{· −} )–scavenging activity. Trypsin peptide (TP) exhibited the highest antioxidative activity compared to other peptide fractions. In considering scavenging effects on hydroxyl radicals (·OH) and Superoxide anions (O₂ ^{· −} ), TP was employed for isolation, purification and identification of antioxidant peptide. To purify and characterize antioxidative peptide, two steps gel filtration, one-step ion-exchange column chromatography and reversed-phase high-performance liquid chromatography (RP-HPLC) were used. The purified antioxidative peptide TP2b-1 was a novel peptide and was sequenced as GPEPTGPTGAPQWLR, in which the low molecular weight and some amino acid constituents played important role in the radical-scavenging effects according reports. The IC₅₀ values of TP2b-1 were 138.9 μM on ·OH and 353.9 μM on O₂ ^{· −} .     

Optimization and Modeling of Process Parameters for Lipase Production by Bacillus brevis

Statistical evaluation of fermentation conditions and nutritional factors by Plackett–Burman two-level factorial design followed by optimization of significant parameters using response surface methodology for lipase production by Bacillus brevis was performed in submerged batch fermentation. Temperature, glucose, and olive oil were found to be the significant factors affecting lipase production. Maximum lipase activity of 5.1 U ml⁻¹ and cell mass of 1.82 g l⁻¹ at 32 h were obtained at the optimized conditions of temperature, 33.7 °C; initial pH, 8; and speed of agitation, 100 rpm, with the medium components: olive oil, 13.73 ml l⁻¹; glucose, 13.98 g l⁻¹; peptone, 2 g l⁻¹; Tween 80, 5 ml l⁻¹; NaCl, 5 g l⁻¹; CH₃COONa, 5 g l⁻¹; KCl, 2 g l⁻¹; CaCl₂·2H₂O, 1 g l⁻¹; MnSO₄·H₂O, 0.5 g l⁻¹; FeSO₄·7H₂O, 0.1 g l⁻¹; and MgSO₄·7H₂O, 0.01 g l⁻¹. The lipase productivity and specific lipase activity were found to be 0.106 U (ml h)⁻¹ and 2.55 U mg⁻¹, respectively. Unstructured kinetic models and artificial neural network models were used to describe the lipase fermentation. The kinetic analysis of the lipase fermentation by B. brevis shows that lipase is a growth-associated product.     

Optimisation of pressurised liquid extraction for antioxidative polyphenolic compound from Momordica charantia using response surface methodology

Pressurised liquid extraction (PLE) of antioxidant compounds from bitter gourd fruits (Momordica charantia) in aqueous ethanolic solvent was investigated using response surface methodology at laboratory scale to understand key impact of extraction variables. Extraction efficiency was optimised by measuring the yield of extraction, total phenolic content (TPC), total flavonoid content (TFC), ferric reducing/antioxidant power assay (FRAP) and radical scavenging activity (RSA). The optimal extraction conditions were reached at 80% ethanol concentration, 10‐min extraction time and at 160 °C. Under these extraction conditions, values of TPC (5.40 ± 0.30 g GAE per 100 g), TFC (1.50 ± 0.10 g QE per 100 g), FRAP (778.55 ± 10 μmol eq Fe (II) g^?1), yield (178.50 ± 5.50 mg g^?1 dc) and RSA (75.50 ± 4.50%) were achieved. Furthermore, statistical analysis revealed that antioxidative attributes of bitter gourd extract were strongly and positively correlated with extraction temperature and ethanol concentration rather than processing time. This study illustrated that PLE has the potential to extract antioxidant compounds from tropical fruit vegetables in an accelerated manner. Furthermore, influential parameters affecting the process could be optimised for further industrial intake.     

A procedure to measure the antiradical efficiency of polyphenols

The kinetic behaviour of polyphenols common in fruits as free radical scavengers was studied using 2,2-diphenyl-1-picrylhydrazyl (DPPH^•). After addi-tion of different standard concentrations to DPPH^· (0·025 g litre⁻¹), the percentage of remaining DPPH^• was determined at different times from the absorbances at 515 nm. The percentage remaining DPPH^• against reaction time followed a multiplicative model equation: ln [DPPH_REM^•]=b ln t+ln a. The slopes of these equations may be useful parameters to define the antioxidant capacity. The steeper the slope, the lower the amount of antioxidant necessary to decrease by 50% the initial DPPH^• concentration (EC₅₀). This parameter, EC₅₀, is widely used to measure antioxidant power, but it does not takes into account the reaction time. Time needed to reach the steady state to the concentration corresponding at EC₅₀ (T_EC50) was calculated, and antiradical efficiency (AE) was proposed as a new parameter to characterise the antioxidant compounds where AE=1/EC₅₀ T_EC50. It was shown that AE is more discriminatory than EC₅₀. AE values are more useful because they also take into account the reaction time. The results have shown that the order of the AE (×10⁻³) in the compounds tested was: ascorbic acid (11·44)>caffeic acid (2·75)⩾gallic acid (2·62)>tannic acid (0·57)⩾DL -α-tocopherol (0·52)>rutin (0·21)⩾quercetin (0·19)>ferulic acid (0·12)⩾3-tert-butyl-4-hydroxyanisole, BHA (0·10)>resveratrol (0·05). © 1998 SCI.     

Extraction of antioxidant and antimicrobial compounds from Inga marginata Willd bark and pulp using different extraction techniques and phytochemical characterization

This study aimed to identify the least aggressive and highest yield extraction method to obtain bioactive compounds from Inga marginata Willd fruits, determine the chemical components, and evaluate the extracts’' antimicrobial and cytotoxic activity. The extraction efficiency was expressed by the total phenolic and total flavonoid content and antioxidant activity (DPPH, IC₅₀, and ORAC) using conventional, ultrasound, and microwave-assisted extraction. The highest bioactive compound content was achieved using 5 min at 60 °C for total phenolic content (214.98 mg GAE g⁻¹), total flavonoid content (22.90 mg EQ g⁻¹), DPPH (45.98 μmol TEAC g⁻¹), inhibitory capacity (0.80 mg mL⁻¹), and ORAC (167.25 μmol Trolox g⁻¹) using ultrasonic extraction, and the extract inhibited the growth of all microorganisms tested. Thirteen chemical compounds were determined by ESI-ToF-MS, confirming the high phytochemical capacity of the extract. Lastly, the Inga extract showed no cytotoxicity at the concentrations used.     

Extraction optimisation,antioxidant activity and inhibition on α-amylase and pancreatic lipase of polyphenols from the seeds of Syzygium cumini

The objectives of this study were to determine the optimal extraction conditions of polyphenols from Syzygium cumini seeds by response surface methodology and investigate their antioxidant activity and inhibition on α-amylase and pancreatic lipase. As results, the optimal extraction conditions in the ultrasonic extraction process which maximised total polyphenols content, minimised the IC₅₀ values of α-amylase and pancreatic lipase were determined as follows: extraction time 60 min, ethanol concentration 63% and solvent/solid ratio 44 mL g⁻¹. The main phenolic compounds in partially purified fraction of Syzygium cumini seeds were catechin, epicatechin, kaempferol, gallic, 5-caffeoylquinic, caffeic and ferulic acids. In addition, the partially purified fraction inhibited 87.66 ± 5.55 and 86.61 ± 3.15% of α-amylase and pancreatic lipase, respectively. The results suggested that Syzygium cumini seeds could be explored as a natural antioxidant and could be used as a source of highly antidiabetic and anti-obesity bioactive compounds.     

Purification,structural data and biological properties of polysaccharide from Prunus amygdalus gum

This work demonstrates the efficiency of almond gum polysaccharides (AGPs) as bioactive compounds. AGPs were first extracted using H₂O₂, in the presence of NaOH, at different times and temperatures. The optimal extraction conditions were 4% H₂O₂ and 2 N NaOH, for 7 h at 50 °C, leading to an extraction yield of 58.2% (w/w). After a purification step, the retained AGPs were characterised using high‐performance liquid chromatography showing a molecular weight of 99.3 kDa. The monosaccharide composition of AGPs were assessed using gas chromatography–mass spectrometry. AGPs were found to be a complex heteropolysaccharide with a repeating unit mainly composed of galactose, arabinose, xylose, mannose, rhamnose, and glucuronic acid with the respective ratios: 45:26:7:10:1:11. The acidic nature of the polysaccharide is due to the presence of glucuronic acid. Total antioxidant activity, free radical‐scavenging activity and reducing power assay of AGPs were investigated. The obtained results showed high antioxidant activities of AGPs. Furthermore, beyond 60 mg mL^?1, AGPs exhibited bacterial growth inhibition for five pathogenic strains: Escherichia coli, Staphylococcus aureus, Enterococcus feacalis, Pseudomonas aeruginosa and Salmonella typhimurium.     

Bioactive compounds and antioxidant activities of Brazilian hop (Humulus lupulus L.) extracts

Bioactive compounds from Brazilian hop (Humulus lupulus L.) cultivars were extracted by ultrasound and their phenolic profile compared with commercial hop from the USA. The most effective extraction conditions (solution of ethanol 49%, at 52 °C and a solid/liquid ratio of 1 g per 34 mL) for the total phenolic compounds (TPC) were determined using a Central Composite Rotatable Design. The Brazilian hop showed higher content of TPC (33.93 ± 0.67 mg GAE g⁻¹), total flavonoids (54.47 ± 0.10 mg QE g⁻¹) and higher antioxidant activity (ABTS: EC₅₀ 21.29 ± 1.36 μL mL⁻¹; DPPH: EC₅₀ 3.91 ± 0.17 μL mL⁻¹) when compared with the USA hop. The main phenolic compounds present in the extracts were the flavonoids isoquercitrin and quercetin. The antioxidant properties of the Brazilian hop extract had not been reported yet in the literature for this raw material, thus showing potential to be incorporated in polymeric films used as active packaging.     

Effect of supercritical CO2 extraction process parameters on oil yield and pigment content from by‐product hemp cake

This research gives an insight into the possibility of exploiting the one of the food industry's by‐products – pressed hemp cake. The complete recovery of oil from pressed hemp cake was achieved. Residual oil that remained in cake after pressing was extracted with supercritical CO₂ by applying different process parameters. Optimal extraction conditions were determined using response surface methodology. Total pigment contents of the oils obtained were determined. Extraction pressure had the most significant influence on yield and pigment content of extracted hemp cake oil. Depending on the pressure, the chlorophyll a content ranged from 101.11 to 378.28 mg kg^?1 and chlorophyll b from 65.14 to 189.78 mg kg^?1, while total carotene content was in the range from 33.58 to 132.67 mg kg^?1. The remaining oil in pressed hemp cake after supercritical CO₂ extraction was determined to be 0.56 ± 0.08% and the defatted cake was rich in proteins and fibre.     

Optimization of supercritical CO2 extraction of phytosterol-enriched oil from Kalahari melon seeds

Supercritical carbon dioxide (SC-CO₂) extraction of oil from Kalahari melon seeds was investigated in this study. Response surface methodology was applied to model and optimize the extraction, namely pressure (200–400 bar), temperature (40–80 °C), and supercritical fluid flow rate (10–20 mL/min). Well-fitting models were successfully established for oil recovery (R ² = 0.9672) and phytosterol concentration (milligrams per 100 g; R ² = 0.8150) through multiple linear regressions with backward elimination. The effect of supercritical fluid flow rate was the most significant (P < 0.05) factor that affected oil recovery but this factor had no significant (P > 0.05) effect on phytosterol concentration. The optimal processing conditions for oil recovery and phytosterol concentration were pressure of 300 bar, temperature at 40 °C, and supercritical fluid flow rate of 12 mL/min. These optimal conditions yielded a 76.3% oil recovery and 836.5 mg/100 g of phytosterol concentration. The oil content in the Kalahari melon seeds as estimated by Soxhlet extraction was around 30.5/100 g. The phytosterol concentration in the oil extracted with SC-CO₂ extraction was 94% higher than that obtained with solvent extraction.     

Efficacy of Acorus calamus L. essential oil as a safe plant‐based antioxidant,Aflatoxin B1 suppressor and broad spectrum antimicrobial against food‐infesting fungi

The study explores the efficacy of Acorus calamus L. essential oil (EO) as a safe plant‐based broad spectrum antifungal, antiaflatoxin, antioxidant food additive. The oil completely inhibited the growth and toxin production of the toxigenic strain of Aspergillus flavus at 0.4 and 0.25 μL mL^?1, respectively. EO exhibited pronounced antifungal activity against sixteen food‐infesting fungal species at 0.5 μL mL^?1. The EO showed strong antioxidant efficacy (IC₅₀ 1.06 μL mL^?1) and nonphytotoxic nature on germination of chickpea seeds. The EO was found nonmammalian toxic showing high LD₅₀ (4877.4 μL kg^?1) for mice (oral, acute). The chemical profile of EO was determined through GC and GC–MS analysis. The findings strengthen the possibility of A. calamus EO as a plant‐based food additive in view of its favourable safety profile, antioxidant and antiaflatoxigenic efficacy and broad spectrum antimicrobial activity against food‐infesting fungi.     

Evaluation of free radical scavenging of dietary carotenoids by the stable radical 2,2‐diphenyl‐1‐picrylhydrazyl

In order to avoid the interference of compounds with a chromophoric system when the 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH^·) method is used, a new measure of the decrease in absorbance at 580 nm was performed (correlation coefficient between absorbance and DPPH^· concentration, 0.9979; p < 0.01). The antioxidant effectiveness of dietary carotenes and xanthophylls towards the stable free radical DPPH^· was measured. The antioxidant activity expressed as the amount of antioxidant able to reduce the initial DPPH^· concentration to 50% (EC₅₀), given in terms of moles of antioxidant per mole of DPPH^·, ranged from 0.16 ± 0.01 (lycopene) to 3.29 ± 0.31 (lutein). The parameter antiradical efficiency (AE), which involves the potency (1/EC₅₀) and the time taken to reach the steady state at EC₅₀ (T_EC50), was calculated to discriminate carotenoids with no significant difference between their EC₅₀. Comparison of the structures of the carotenoids tested revealed that the scavenging ability towards DPPH^· was increased by the length of the effective conjugated double‐bond system and was modulated by the addition of chemical groups on the terminal rings (xanthophylls). © 2000 Society of Chemical Industry