Optimization Of Extraction Parameters Research Articles

Parrotia persica as a Potential Source of Bioactive Phenolic Compounds: Optimization of Extraction Parameters and Biological Activity Assay

Parrotia persica is one of the endemic plants in Iran and belongs to the Hamamelidaceae family. A wide range of biological activities of this plant have been attributed to several phenolic compounds. In this study, the phenolic bioactive compounds extraction from P. persica leaves was performed using conventional and ultrasonic‐assisted extraction (UAE) techniques through the response surface methodology (RSM) to optimize the best extraction conditions and reach the maximum amount of phenolic compounds. The central composite design (CCD) was conducted for the optimization of four extraction parameters, including extraction time, alcohol concentration, solvent‐to‐solid ratio, and temperature. The coding of parameters was performed as an independent variable at five levels. Quantitative and qualitative assessments were achieved by using HPLC, LC‐MS, and UV‐Vis spectrophotometry. According to the results, UAE was chosen as the best method with the optimal extraction values: 15 min as an extraction time, 40% alcohol portion in solvent, solvent‐to‐solid ratio equal to 30 : 1, and 25°C for temperature. In this regard, it was found that the similarity of experimental to predicted findings was 98.7% for the phenolic content and 94.9% for the mass extract in the UAE method. The findings showed a good similarity between the experimental and predicted values, and no significant changes were observed between the real and theoretical results. In addition, our finding revealed that the optimum extraction yield was 28.5% for the mass extract in the UAE optimization process. Furthermore, the antioxidant activity by DPPH assay indicates that the extract which was obtained using UAE in optimum condition, proposed remarkable antioxidant activity (IC50 29.86 μg·ml−1). Moreover, the cytotoxic assay was performed against PC‐3 cancer cells, and it was found that the optimized extract using UAE has a promising cytotoxic activity (IC50 10.4 μg·ml−1) without toxicity toward normal cells. Since there is a possibility to use P. persica as one of the commercial herbal sources, the optimized extraction models could be utilized for scaling up the phenolic compound extraction from P. persica leaf.

Response surface methodology-optimized extraction of flavonoids from pomelo peels and isolation of naringin with antioxidant activities by Sephadex LH20 gel chromatography

In this study, flavonoids were extracted from pomelo peels and naringin was isolated from the flavonoid extract. The effects of extraction parameters, namely, ethanol concentration, solid-to-liquid ratio, and extraction time, on the yield of flavonoids extracted from pomelo peels were analyzed according to the Box-Behnken design of response surface methodology. The experimental conditions for flavonoid extraction were optimized, and naringin was separated from the extracted flavonoids using Sephadex LH-20 column chromatography. Experimental results showed that the influence of factors on the extraction rate of flavonoids from pomelo peels was in the order of ethanol concentration > solid-to-liquid ratio > extraction time, and the optimal extraction parameters were 85% ethanol concentration, 1:20 solid-to-liquid ratio, and 4-h extraction time for extracting flavonoids from pomelo peels. Under these conditions, the yield of flavonoids was 6.07 ± 0.06 mg/g. After three times of extraction, the flavonoid extraction rate reached 96.55%, and the residual naringin in the pomelo peels was 0.017 mg/g, at which point the bitterness in the pomelo peels disappeared. Two components, namely, PF1 and PF2, were separated from the crude flavonoid of pomelo peels through Sephadex LH20 column chromatography. PF2 was identified as naringin by high-performance liquid chromatography tandem mass spectrometry, with a purity of 95.7 ± 0.23%. Both flavonoids and PF2 exhibited good in vitro radicals scavenging activities on DPPH, ABTS, superoxide anion and hydroxyl.

Preparation of a single and reusable biopolymer-based film for the extraction and preconcentration of anti-inflammatory drugs from environmental water samples.

One of the main goals of green chemistry is to reduce the use of toxic materials and the generation of hazardous waste, both during method development and in the synthesis of the materials used. Thus, a biodegradable, single and reusable material composed of agarose and multi-walled carbon nanotubes was proposed. The film preparation was carefully optimized in order to obtain a one-piece sorbent, with high extraction efficiency and the possibility of reuse. The film was tested in the simultaneous extraction and preconcentration of three non-steroidal anti-inflammatory drugs (ketorolac, ketoprofen and piroxicam) from environmental water samples. The optimal extraction parameters were as follows: isopropyl alcohol as the activation solvent, a sample pH value of 3.0, extraction time of 30 min, 2.00 mL of acetonitrile as the eluent, an elution time of 5 minutes, and a sample volume of 250.00 mL. Under these conditions, the film was reusable 50 times without losing its extraction capacity significantly. HPLC with a photodiode array detector was used for the separation and determination. The method presented a linear range between 0.10 and 1.2 μg L-1, good sensitivity with limits of detection between 0.0075 and 0.0089 μg L-1, and quantification between 0.025 and 0.030 μg L-1. In addition, low RSD values (0.46-3.13%) were obtained demonstrating satisfactory precision. Stream water samples were analyzed, and recoveries between 82.0 and 109.0% were obtained.

Chemical Compositions, Extraction Optimizations, and In Vitro Bioactivities of Flavonoids from Perilla Leaves (Perillae folium) by Microwave-Assisted Natural Deep Eutectic Solvents.

Natural deep eutectic solvents (NADESs) have been gradually applied to green extraction of active ingredients. In this study, microwave-assisted NADESs were applied to the extraction of flavonoid compounds from perilla leaves. Through comparative experiments, NADES-3 (choline chloride and malic acid at a molar ratio of 1:1) was found to have the highest extraction efficiency of total flavonoids, including apigenin 7-O-caffeoylglucoside, scutellarein 7-O-diglucuronide, luteolin 7-O-diglucuronide, and scutellarein 7-O-glucuronide by HPLC-MS. The following optimal extraction parameters were obtained based on response surface design: water content in NADES of 23%, extraction power of 410 W, extraction time of 31 min, and solid-liquid ratio of 75 mg/mL, leading to the extraction yield of total flavonoids of 72.54 mg/g. Additionally, the strong antimicrobial and antiallergic activity, inhibition of nitrosation, and antioxidant activity of total flavonoids by using NADESs were confirmed. This new extraction method provides a reference for the further exploration of NADES systems and may be widely used for the green extraction of natural active ingredients.

Optimization of Solvent Extraction of Lipids from Yarrowia lipolytica towards Industrial Applications

Extraction of intracellular lipids of the oleaginous yeast Yarrowia lipolytica has been systematically studied aiming towards a sustainable extraction process for lipid recovery. Selection of suitable industrial (bulk) solvents and extraction parameters that lead to maximization of lipid recovery are significant issues to be addressed, with industrial applications motivating this study. Biomass from fermentation of Yarrowia lipolytica (MUCL 28849) was used in small laboratory tests to assess different solvent mixtures (i.e., methanol/hexane, isopropanol/hexane, and methanol/ethyl acetate), implementing a systematic design of experiments methodology to identify near-optimum values of key extraction variables (i.e., polar/non-polar ratio, vortex time, dry biomass/solvent ratio) in regard to lipid yield (g lipids/g dry biomass). The methanol/hexane mixture exhibited the highest extraction yield in a wide range of experimental conditions, resulting in the following optimum parameters: polar/non-polar ratio 3/5, vortex time 0.75 h, and dry biomass/solvent ratio 40. Extraction tests on a fifty-times-larger scale (in a Soxhlet apparatus employing the optimal extraction parameters) confirmed the optimization outcome by obtaining up to 27.6% lipids per dry biomass (L/DB), compared to 12.1% L/DB with the reference lipid extraction method employing chloroform/methanol. Assessment of lipid composition showed that unsaturated fatty acid recovery was favored by the methanol/hexane solvent. Fatty acid composition was not affected by the increase in Soxhlet reflux cycles, whilst the lipid yield was notably favored.

Extraction and Purification of Flavonoids from Buddleja officinalis Maxim and Their Attenuation of H2O2-Induced Cell Injury by Modulating Oxidative Stress and Autophagy.

Cataracts are an ailment representing the leading cause of blindness in the world. The pathogenesis of cataracts is not clear, and there is no effective treatment. An increasing amount of evidence shows that oxidative stress and autophagy in lens epithelial cells play a key role in the occurrence and development of cataracts. Buddleja officinalis Maxim flavonoids (BMF) are natural antioxidants and regulators that present anti-inflammatory and anti-tumor effects, among others. In this study, we optimized the extraction method of BMFs and detected three of their main active monomers (luteolin, apigenin, and acacetin). In addition, a model of oxidative damage model using rabbit lens epithelial cells induced by hydrogen peroxide (H2O2). By detecting the levels of superoxide dismutase (SOD), glutathione peroxidase (GSH-Px), malondialdehyde (MDA), and OH (OH), the expression of autophagosomes and autolysosomes were observed after MRFP-GFP-LC3 adenovirus was introduced into the cells. Western blotting was used to detect the expression of Beclin-1 and P62. Our research results showed that the optimal extraction parameters to obtain the highest yield of total flavonoids were a liquid−solid ratio of 1:31 g/mL, an ethanol volume fraction of 67%, an extraction time of 2.6 h, and an extraction temperature of 58 °C. Moreover, the content of luteolin was 690.85 ppb, that of apigenin was 114.91 ppb, and the content of acacetin was 5.617 ppb. After oxidative damage was induced by H2O2, the cell survival rate decreased significantly. BMFs could increase the levels of superoxide dismutase (SOD) and glutathione peroxidase (GSH-Px) and decrease the levels of malondialdehyde (MDA) and OH (OH). After the MRFP-GFP-LC3 virus was introduced into rabbit lens epithelial cells and detecting the expression of P62 and Beclin-1, we found that the intervention of BMF could promote the binding of autophagosomes to lysosomes. Compared with the model group, the level of P62 in the low-, middle-, and high-dose groups of BMF was significantly down-regulated, the level of Beclin-1 was significantly increased, and the difference was statistically significant (p < 0.05). In other words, the optimized extraction method was better than others, and the purified BMF contained three main active monomers (luteolin, apigenin, and acacetin). In addition, BMFs could ameliorate the H2O2-induced oxidative damage to rabbit lens cells by promoting autophagy and regulating the level of antioxidation.

Extraction Optimization of Crocin from Gardenia (Gardenia jasminoides Ellis)Fruits Using Response Surface Methodology and Quality Evaluation of Foam-Mat Dried Powder

The crocin in gardenia, as a medical plant, has drawnthe attention of researchers and scientists due to its color and high antioxidant activity. To optimize the extraction parameters of crocin from gardenia fruits, response surface methodology (RSM) was employed.The effects of four independent variables, namely extraction temperature (45–55 °C), time (40–60 min), percentage of gardenia fruits(15–25%), and ethanol concentration (50–60%),on a crocin compound were investigated. The extract from the gardenia fruit was dried at different temperatures (55–70 °C) by the foam-mat drying method. The optimal extraction parameters were an extraction temperature of 55 °C, time of 57 min, percent of fruits in solvent at 24%, and an ethanol concentration of 56%. The results showed that the dried gardenia powder had maintained the crocin content well(6.64 mg/g), and the product with low water activity and moisture content of 0.33 and 5.72%, respectively, is suitable for storage. The foam-mat dried product also maintains the natural color and characteristics inherent in the raw materials, which could also be used as supplemental ingredients for other food industries.

Optimization of Extraction Parameters and Characterization of Tunisian Date Extract: A Scientific Approach Toward Their Utilization.

The online version contains supplementary material available at 10.1007/s12355-022-01223-2.

Optimization of Extraction Conditions and Cytotoxic Activity of Rapanone in Comparison to Its Homologue, Embelin.

Rapanone is a plant-derived simple alkyl-dihydroxybenzoquinone structurally close to embelin, a well-known cytotoxic agent. The pharmacological characterization of rapanone is still incomplete, and to fill the data gap, a good source for its acquisition is required to conduct further research. This study aimed to optimize the conditions for the extraction of rapanone from the leaves of white-berried Ardisia crenata Sims. For this purpose, three methods were employed: heat reflux (HRE), shaking (SE), and ultrasound-assisted extraction (UAE), and such parameters as the extraction time, solvent, and the number of extractions from the same sample were set as experimental variables. Furthermore, cytotoxic activity toward prostate cancer, thyroid cancer, and colorectal carcinoma cell lines was investigated and compared with doxorubicin and embelin. The most effective and economical method for the extraction of rapanone was shown to be 20 min UAE with ethyl acetate or chloroform. Rapanone exhibited high cytotoxic activity against PC3 (IC50 = 6.50 μg/mL), Du145 (IC50 = 7.68 μg/mL), FTC133 (IC50 = 6.01 μg/mL), 8505C (IC50 = 7.84 μg/mL), and Caco-2 (IC50 = 8.79 μg/mL) cell lines after 24 h and against the HT29 cell line after 48 h (IC50 = 11.67 μg/mL). Furthermore, it revealed a more favorable safety profile than either its homologue, embelin, or doxorubicin. The set of optimal extraction parameters obtained may be utilized for scientific and industrial purposes to achieve the best rapanone yield. Moreover, this benzoquinone revealed a high cytotoxic activity with good selectivity.

Resource-saving melon processing technology

The object of the study is the fruits of melon. The problem is the crop that remains in the fields. The article provides an overview of technologies for the processing of melons, and studies of the authors are given. On the basis of these studies, technological schemes for the production and formulation of such products as jam, jam, confiture, blended juices, vegetable oil from melon seeds were proposed and justified. Optimal additives and ways of introducing pectin into them are determined. The presence in finished products of vitamins of group B, vitamin C, β-carotene, almost all essential amino acids, micro- and macroelements, the content of which does not noticeably decrease during storage under the optimal conditions established by us. Studies have been carried out on the selection of an extractant and the determination of the optimal parameters for extraction, isolation, neutralization and drying of pectin from melon peel. As a result, pectin was obtained with a degree of esterification of 67...69 %, a jelly-forming ability of more than 170 degrees of Tarr Baker, and a jelly strength of about 460 mm Hg

In Vitro Bioactivities of Food Grade Extracts from Yarrow (Achillea millefolium L.) and Stinging Nettle (Urtica dioica L.) Leaves

Yarrow (Achillea millefolium L., AM) and nettle (Urtica dioica L., UD) are bioactive plants used commercially in functional food and supplement applications and traditionally to alleviate gastric disorders. In this work, the effects of food-grade optimized extracts of Finnish early-season AM and UD were tested on bacterial growth including potential beneficial and foodborne pathogens, as well as murine norovirus (MNV). The anti-inflammatory properties of the extracts were also tested in vitro by NF-κB reporter cells. The food-grade extraction was optimized with the response surface modelling in terms of total carotenoid, chlorophyll, and phenolic compounds contents and antioxidant capacities. The optimal food-grade extraction parameters were a 1-h extraction in 70% ethanol at 45 °C for AM, and at 49 °C for UD. There were no significant effects on the beneficial bacteria (Lacticaseibacillus and Bifidobacterium strains), and the extracts were more effective against gram-positive than gram-negative foodborne bacteria and potential pathogens. Listeria innocua was the most susceptible strain in the optimized extracts with a growth rate of 0.059 ± 0.004 for AM and 0.067 ± 0.006 for UD, p < 0.05 compared to control. The optimized extracts showed a logarithmic growth reduction of 0.67 compared to MNV. The hydroethanolic extracts were cytotoxic to both cell lines, whereas aqueous AM and UD extracts induced and reduced TLR4 signalling in a reporter cell line, respectively. The results provide novel food-grade extraction parameters and support the bioactive effects of AM and UD in functional food applications, but more research is needed to elucidate the precise biological activity in vivo for gastric health.

Optimization of Pulsed Electric-Field-Based Total Polyphenols’ Extraction from Elaeagnus pungens ‘Limelight’ Leaves Using Hydroethanolic Mixtures

In this study, the use of pulsed electric field (PEF) for the extraction of polyphenols from mature Elaeagnus pungens ‘Limelight’ leaves is discussed. Optimization of the main parameters that affect the extraction process was carried out. More specifically, the composition of the solvent (ethanol, water, and mixtures of the two at a 25% v/v step gradient) and the main PEF-related parameters (i.e., pulse duration, pulse period, and electric field intensity) was optimized. The obtained extracts were examined for their polyphenol content with the Folin–Ciocalteu assay and individual polyphenols were also assessed with high-performance liquid chromatography. The extracts obtained with PEF were compared to the extract compared without PEF, in terms of total polyphenols. According to the results, the optimum extraction parameters were found to be a pulse duration of 10 μs, a pulse period of 1000 μs, and an electric field intensity of 0.85 kV cm−1 after 20 min of extraction. The optimum solvent was found to be the 50% (v/v) ethanol/water mixture. The extract prepared under the optimum conditions was found to contain 58% more polyphenols compared with the extract prepared without PEF. Moreover, an increase of up to 92% was recorded for specific polyphenols. Based on the above, it was evidenced that the examined parameters influenced the recovery of polyphenols, suggesting that such parameters should be also examined in similar studies, in order to maximize the extraction yield of polyphenols.

Revitalizing Unfermented Cabernet Sauvignon Pomace Using an Eco-Friendly, Two-Stage Countercurrent Process: Role of pH on the Extractability of Bioactive Phenolics

As the major byproduct of the winemaking industry, grape pomace remains an untapped source of valuable bioactive phenolic compounds. This study elucidated the optimal aqueous extraction parameters for maximizing phenolic extractability, while avoiding the use of harsh conventional solvents and limiting water usage, from Cabernet Sauvignon grape pomace in which the red grape was processed for white wine. In the single-stage aqueous extraction process (AEP), the concurrent impact of pH (2.64–9.36), solids-to-liquid ratio (SLR, g pomace/mL water) (1:50–1:5), and temperature (41.6–58.4 °C) on the total phenolic content (TPC) of Cabernet Sauvignon pomace was evaluated alongside a kinetic study (15–90 min). Optimal single-stage extraction conditions (pH 9.36, 1:50 SLR, 50 °C, 75 min) guided the development of a two-stage countercurrent extraction process (pH 9.36, 1:10 SLR, 50 °C, 75 min) to further reduce water consumption without compromising overall extractability. The countercurrent process reduced fresh water usage by 80%, increased the TPC of the extracts by 18%, and improved the in vitro antioxidant activities (ABTS and ORAC) of the extracts. Untargeted metabolomics enabled the identification of a diverse pool of phenolics, especially flavonol glycosides, associated with grape pomace, while further phenolic quantitation detected improvements in the release of commonly bound phenolics such as ferulic acid, p-coumaric acid, syringic acid, and protocatechuic acid in alkaline extracts compared to the ethanolic extract. This investigation provides an efficient, eco-friendly extraction strategy suitable for applications in functional food, beverage, nutraceutical, and cosmetic industries.

Optimization of ultrasound-assisted extraction of phenolic content & antioxidant activity of hog plum (Spondias pinnata L. f. kurz) pulp by response surface methodology

BackgroundThe pulp of hog plum (Spondias pinnata L. f. kurz) has been documented as a potential source of nutritional, physiological, and pharmacological purposes due to its phenolic content (TPC) and antioxidant activity. However, an optimal extraction condition for hog plum pulp remains elusive. Optimization of extraction process conditions using Ultrasound-assisted extraction (UAE) technique has recently attracted research interest. ObjectivesThe present study focused on optimizing the UAE extraction conditions of TPC and antioxidant activities (DPPH and FRAP) from hog plum pulp by using response surface methodology (RSM). MethodsThe RSM with a three-factor-three-level Box-Behnken design (BBD) was used to optimize the extraction conditions. The BBD was used to investigate the effects of three independent variables, X1: ultrasonic temperature (40–60 °C), X2: ultrasonic time (30–60 min), and X3: ethanol concentration (40–80%) on TPC, DPPH and FRAP assays. Fifteen experimental trials have been carried out to optimize the UAE extraction conditions. A second-order polynomial model was used for predicting the responses. Statistically, the model was validated using an analysis of variance (ANOVA). ResultsThe ANOVA results revealed that UAE extraction temperature, time, and ethanol concentration had a significant (p < 0.01) influence on the TPC, DPPH, and FRAP, suggesting that all extraction parameters included in this investigation were crucial to the optimization process. For TPC, DPPH, and FRAP, the R2 values were 0.9976, 0.9943, and 0.9989, respectively, indicating that the models developed based on second-order polynomials were satisfactorily accurate for analyzing interactions between parameters (response and independent variables). RSM analysis showed that the optimal extraction parameters which maximized TPC, DPPH, and FRAP were 52.03 °C temperature, 30 min, time, and 79.99% ethanol. Under optimal conditions, experimental values for TPC, DPPH, and FRAP were 370 ± 26 mg GAE/100g DM, 57 ± 7%, and 7650 ± 460 mg AAE/100 g DM, respectively. The experimental values showed a good agreement with the predicted values with residual standard error values below 0.2% under optimum conditions. Pearson's correlation coefficients (r) demonstrate that the TPC showed a weak positive correlation with DPPH (r = 0.3508) and moderate correlation with FRAP (r = 0.3963). ConclusionThe experimental results agreed with the predicted values, confirming the model's appropriateness and RSM's efficacy in optimizing the UAE extraction conditions. This optimized UAE extraction method may be effective in the industrial extraction process; moreover, further research should be conducted to determine the efficacy of these extracts when applied to food.

REGRESSION ANALYSIS IN DEVELOPMENT OF PROCEDURE FOR ISOLATION AND QUANTITATIVE DETER-MINATION OF WATER-SOLUBLE POLYSACCHARIDES FROM DANDELION ROOTS OF MEDICINAL

The roots of the dandelion drug (Taraxacum officinale F.H. Wigg) are rich in chemical composition and contain water-soluble polysaccharides based on inulin. The aim of the study is to select optimal parameters of ultrasonic extraction of water-soluble polysaccharides from dandelion roots based on regression analysis. For the experiment, raw materials purchased from one of the pharmacies in the city of Voronezh were used. A sample of raw materials (1.0 g) was placed in an ultrasonic bath "Grad 40-35," which allows maintaining the necessary temperature and frequency of ultrasound with a given duration of time. one-year old, as well as in industrial production of water-soluble polysaccharides from this kind of raw material. Then, 10 (15 or 20) ml of purified water purified from impurities at a temperature of 60 °C to 80 °C was measured with a measuring flask and extracted from 10 to 20 min with a multiplicity of 1 to 3, and after each of the multiple studies, the same raw material was further filtered with a new solvent. The initial conditions and the data obtained during the experiments made it possible to present the regression model in the form of a linear multiple regression equation, which can be used with sufficient accuracy in prediction and analysis. The adequacy of the model was confirmed by testing hypotheses against Pearson's x2 criterion. The correlation coefficient derived from the values of the regression coefficient and the mean square deviation was used in determining the tightness of the overall relationship between the source and the obtained data. In addition, a detailed study of a sample of those variables whose priority was not clearly expressed was carried out by processing when fixing their values. The most important conditions for extraction of dandelion roots for obtaining the most stable performance should be considered: extraction temperature – 80 °C; extraction multiplicity – 3, ultrasound frequency – 35 kHz, extraction time – 40 min, ratio of raw material and extractant – 1 g per 10 ml, at the same time, grinding of raw material can vary from 0.2 mm to 0.5 mm.

Green extraction and separation of Dendranthema indicum essential oil by supercritical carbon dioxide extraction combined with molecular distillation

The optimal extraction parameters of Dendranthema indicum extract using supercritical carbon dioxide extraction were organized by response surface methodology (RSM) with Box - Behnken design (BBD). The peak extraction yield (9.37%) was obtained in the condition of 750 W of microwave power, 40 °C of extraction temperature, 26 MPa of extraction pressure, and 105 min of extraction time. Subsequently, molecular distillation was applied to separate essential oil from D. indicum extract. The separation yield of D. indicum essential oil obtained at 80 (DIEO80) and 90 °C (DIEO90) were 0.21 g/100 g and 0.44 g/100 g, respectively, which was lower than those of 100, 110 and 120 °C, while they presented transparent with no precipitate. DIEO90 possessed the strongest antioxidant activities (16.08 μmol TE/g for 1,1-diphenyl-2-picrylhydrazyl scavenging activity, 46.05 μmol TE/g for ferric reducing antioxidant power, respectively). Furthermore, alkenes, alcohols and esters were identified the main volatile flavor components for D. indicum extract and essential oils. The proportions of major contributing components such as 1,8-cineol (6.45%–15.04%), isopinocarveol (6.02%–11.78%), (E)-α-bergamotene (3.02%–5.62%), (E)-β-famesene (2.80%–12.92%), germacrene D (2.83%–8.23%), 6-ethenyl-2,2,6-trimethyloxan-3-ol (5.86%–6.88%), (6-Ethenyl-2,2,6-trimethyl-oxa- n-3-yl) acetate (9.11%–10.51%) and β-elemene (4.16%–6.44%). Though molecular distillation, compounds with low boiling points were enriched in DIEO80 and DIEO90, and compounds with high boiling points were in other oils. Overall, the sequential green process based on supercritical carbon dioxide extraction with molecular distillation is an efficient method for extraction and separation of essential oil.

Optimization of ethanol based extraction of phenolics from Ocimum sanctum flowers by response surface methodology

Ocimum sanctum L. flowers have been reported to have various health benefits owing to its phenolic composition. However, the available phenolic compounds should be effectively extracted to efficiently utilize these flowers. This study was aimed to make use of response surface methodology (RSM), to simultaneously optimize the process parameters to obtain maximum yield of phenolics and anthocyanins along with maximum DPPH radical scavenging activity from O. sanctum flowers. Central composite design (CCD) was employed with four independent variables; solid:liquid ratio (XA), ethanol concentration (XB), temperature (XC) and time (XD) which were found to affect the response variables significantly and fit to the second order polynomial model. The results showed that the polynomial models for all responses were significant (p < 0.05) and did not show lack of fit and presented acceptable coefficients of determination. This indicates the suitability of the models for prediction purposes. The desirability function approach in the scale of 0–1 was used to determine the optimized conditions. The optimum process parameters obtained were XA; 1:35 (w/v), XB; 55%, XC; 44 °C and XD; 32 min. The experimental values obtained based on optimum extraction parameters agreed with the predicted values. The findings suggests the application of optimized parameters to acquire functionally active phenolics and anthocyanins from O. sanctum flowers using ethanol and make use of them in food and pharmaceutical industry.

Protic ionic liquids based on anionic clusters ([Hmim][(HSO4)(H2SO4]x) with (x = 0, 1, and 2), to produce nanocellulose (CNC)

This work deals with the production of crystalline nanocellulose (CNC) through an acid hydrolysis reaction using protic ionic liquids (PILs) as solvents and catalysts. The PILs used belong to a series derived from a common cation, 1-methyl- imidazolium and anionic clusters of the general formula [(HSO4)(H2SO4)x]− (x = 0, 1, 2). These PILs were used for the first time to obtain CNC from two commercial cellulose samples and one cellulose from a corn husk source. The PILs were used under different time and temperature conditions to set the optimal parameters for extraction. The CNCs obtained were characterized by IR spectroscopy, X-ray diffraction spectroscopy, STEM and FESEM microscopy and thermal stability by thermogravimetric analysis (TGA). It was determined that the [Hmim][(HSO4)(H2SO4)x] with x = 1 presents the appropriate acidity, (measured by Hammett acidity function (H0) and acceptor number (AN) parameters), to extract CNC from two different commercial cellulose with a yield of ca 73 % and 60% (at 40 °C with 2–3 h of reaction); respectively. The experimental conditions used in this study (time and 40 °C) are milder than those reported when sulfuric acid and other ILs were used to obtain CNC. The [Hmim][(HSO4)(H2SO4)x] with x = 1 present an adequate acidity for the selective water-insoluble oligosaccharides release, while products resulting from 64% sulfuric acid (H0 = 0.65) at 40 °C were mainly water-soluble oligosaccharides.Additionally, the PILs were recycled 5 times maintaining their original structural and catalytic properties. The proposed process was also compared with a conventional acid hydrolysis using sulfuric acid (64 wt%), the nanomaterial obtained with the PILs always presented better thermal properties. This work contributes towards the use of new solvents-catalysts in the field of biomass waste recovery under mild reaction conditions.

Optimization Extraction of Cladonia foliacea (Huds.) Willd: Antioxidant Activity and Inhibition of the Key Enzymes Linked to Type II Diabetes

Cladonia foliacea (CF) is a type of lichen belonging to the Cladoniaceae family, used as traditional medicine for various diseases. It is known that CF has strong antioxidant and antidiabetic effects originating from various secondary components. However, the bioactivity of CF is significantly affected by extraction conditions such as temperature, liquid/solid ratio, and solvent type/concentration. Herein, the extraction parameters (temperature, liquid/solid ratio, and methanol concentration) of CF were optimized by response surface methodology (RSM) based on maximum total phenolic content (TPC), antioxidant capacity, and α-glucosidase/α-amylase inhibitor activity. In the methanolic extraction of CF, 48.8 °C, 12.3 mL g-1 liquid/solid ratio, and 86.4% methanol concentration were determined as the optimum point. TPC, antioxidant capacity, α-glucosidase, and α-amylase inhibition activities of CF extracted under optimum conditions were determined as 5.55 mg GAE g-1, 33.10 g sample/g DPPH, 68.78%, and 50.03%, respectively. These results suggest that extraction conditions may be a limiting factor in terms of bioactive properties and optimized extraction parameters may improve the potential antioxidant and inhibitory activity of key enzymes associated with type II diabetes of CF.

Surfactant‐assisted extraction of Melaleuca alternifolia (tea tree) oil by hydrodistillation and its application in microemulsion

AbstractBACKGROUNDThe surfactant‐assisted extraction of essential oils from Melaleuca alternifolia foliage, also known as tea tree oil (TTO), was systematically studied with the design of experiments (DoE) aiming to improve the extraction of TTO. Specifically, the optimal parameters of hydrodistillation process were obtained with the response surface methodology (RSM) based on a central composite design (CCD).RESULTSThe concept of enhanced TTO extraction with the renewable nonionic Triton CG‐110 surfactant was proven. An optimal extraction yield of TTO was predicted by the RSM model at 6.71 wt% under the following conditions: (i) 597 mg L−1 Triton CG‐110 as liquid extractant, (ii) a ratio of liquid extractant/desiccated leaf at 25.4 mL g−1, and (iii) 140 min for the extraction time. The presence of 650 mg L−1 Triton CG‐110 in the extractant could increase the extraction rate of TTO by 17.5%, compared to that without surfactant. The forecast of the DPPH antioxidant activity of TTO by RSM was in good accordance with the measured values. Various microemulsion formulations of TTO with Triton CG‐110 were developed and reported.CONCLUSIONThe presence of a proper surfactant in the liquid extractant can improve the extraction of essential oils, not only in the form of yield but also in the rate of extraction. No trace of surfactant could be found in the produced essential oil because of the relatively higher boiling point and the lower volatility of the surfactant. The RSM was successfully applied to obtain the optimal extraction parameters for tea tree oil by the surfactant‐enhanced hydrodistillation process. © 2022 Society of Chemical Industry (SCI).