Physicochemical,Thermal and Rheological Properties of Pectin Extracted from Sugar Beet Pulp Using Subcritical Water Extraction Process

The objective of this study was to characterize the properties of pectin extracted from sugar beet pulp using subcritical water (SWE) as compared to conventional extraction (CE). The research involved advanced modeling using response surface methodology and optimization of operational parameters. The optimal conditions for maximum yield of pectin for SWE and CE methods were determined by the central composite design. The optimum conditions of CE were the temperature of 90 °C, time of 240 min, pH of 1, and pectin recovery yield of 20.8%. The optimal SWE conditions were liquid-to-solid (L/S) ratio of 30% (v/w) at temperature of 130 °C for 20 min, which resulted in a comparable yield of 20.7%. The effect of obtained pectins on viscoamylograph pasting and DSC thermal parameters of corn starch was evaluated. The contents of galacturonic acid, degree of methylation, acetylation, and ferulic acid content were higher in the pectin extracted by SWE, while the molecular weight was lower. Similar chemical groups were characterized by FTIR in both SWE and CE pectins. Color attributes of both pectins were similar. Solutions of pectins at lower concentrations displayed nearly Newtonian behavior. The addition of both pectins to corn starch decreased pasting and DSC gelatinization parameters, but increased ΔH. The results offered a promising scalable approach to convert the beet waste to pectin as a value-added product using SWE with improved pectin properties.     

In-Vitro Screenings for Biological and Antioxidant Activities of Water Extract from Theobroma cacao L. Pod Husk: Potential Utilization in Foods

Increasing production of cocoa (Theobroma cacao L.) leads to a higher environmental burden due to its solid waste generation. Cocoa pod husk, one of the major solid wastes of cocoa production, contains rich bioactive compounds unveiling its valorization potential. With that in mind, our research aimed to explore the biological and antioxidant activities of aqueous extracts from cocoa pod husks. In this present work, cocoa pod husk was extracted using water and subsequentially partitioned using n-hexane, ethyl acetate, and methanol. The antimicrobial investigation revealed that the ethyl acetate solubles were active against the Staphylococcus aureus, Escherichia coli, and Candida albicans, where at a 20% w/v concentration, the inhibition diameters were 6.62 ± 0.10, 6.52 ± 0.02, and 11.72 ± 0.36 mm, respectively. The extracts were found non-toxic proven by brine shrimp lethality tests against Artemia salina with LC₅₀ scores ranging from 74.1 to 19,054.6 μg/mL. The total phenolic content and total flavonoid content were obtained in the range of 47.44 to 570.44 mg/g GAE and 1.96 to 4.34 mg/g QE, respectively. Antioxidant activities of the obtained extracts were revealed by 2,2-diphenyl-1-picryl-hydrazyl-hydrate (DPPH) assay with EC₅₀ reached as low as 9.61 μg/mL by the ethyl acetate soluble. Phytochemical screening based on gas chromatography—mass spectroscopy analysis on the sample with the highest antioxidant activities revealed the dominant presence of three phytosterols, namely gamma-sitosterol, stigmasterol, and campesterol.     

Isolation,Chemical Characterization and Antioxidant Activity of Pectic Polysaccharides of Fireweed (Epilobium angustifolium L.)

The aim of this study was to isolate pectins with antioxidant activity from the leaves of Epilobium angustifolium L. Two pectins, EA-4.0 and EA-0.8, with galacturonic acid contents of 88 and 91% were isolated from the leaves of E. angustifolium L. by the treatment of plant raw materials with aqueous hydrochloric acid at pH 4.0 and 0.8, respectively. EA-4.0 and EA-0.8 were found to scavenge the DPPH radical in a concentration-dependent manner at 17–133 μg/mL, whereas commercial apple pectin scavenged at 0.5–2 mg/mL. The antioxidant activity of EA-4.0 was the highest and exceeded the activity of EA-0.8 and a commercial apple pectin by 2 and 39 times (IC₅₀—0.050, 0.109 and 1.961 mg/mL), respectively. Pectins EA-4.0 and EA-0.8 were found to possess superoxide radical scavenging activity, with IC₅₀s equal to 0.27 and 0.97 mg/mL, respectively. Correlation analysis of the composition and activity of 32 polysaccharide fractions obtained by enzyme hydrolysis and anionic exchange chromatography revealed that the antioxidant capacity of fireweed pectins is mainly due to phenolics and is partially associated with xylogalacturonan chains. The data obtained demonstrate that pectic polysaccharides appeared to be bioactive components of fireweed leaves with high antioxidant activity, which depend on pH at their extraction.     

Emulsifying properties and functional compositions of sugar beet pectins extracted under different conditions

Extraction conditions have important effects on the characteristics of sugar beet pectin (SBP). Response surface methodology (RSM) was used to study the impact of different extraction parameters on pectin yield, protein, ferulic acid, and galacturonic acid contents as well as on the emulsifying properties. Results indicated that pH was the main factor influencing pectin yield (ranging from 6.7 to 24.6%). Protein content varied from 0.5 to 6%, while ferulic acid content (ranging from 1.55 to 2.42%) was slightly influenced by the extraction conditions. Droplet sizes of the emulsions stabilized by different SBPs varied from 1.12 to 4.12 µm. Furthermore, according to the correlation analysis, protein content–pectin yield and ferulic acid–pectin yield demonstrated good correlations, respectively. Based on the present study, SBP with different functional components could be extracted as per relevant practical objectives.     

Supercritical carbon dioxide extraction of Usnea longissima (L.) Ach.: Optimization by Box-Behnken design (BBD)

Usnic acid (UA) was extracted from Usnea longissima (L.) Ach. in supercritical carbon dioxide (SC-CO₂) medium. The selected process parameters were extraction temperature (35–45 °C), amount of co-solvent (0%–5%) and extraction time (5–9 h). These parameters were applied to Box-Behnken design (BBD) belonging to response surface methodology (RSM) to determine optimum process parameters for the highest amount of UA in the extract. g UA/100g lichen, extraction yield % and UA content values were calculated in the range of 0.045–0.317, 2.77–5.4 and 71%–82% in different experimental conditions, respectively. The optimum conditions were predicted as 42 °C, 4.3% (ethanol) and 7.48 h. It was determined that the predicted and experimental values of g UA/100g lichen were compatible, and the suggested model was valid.     

Polysaccharides ofEremurus. XXI. Pectin substances of the leaves ofEremurus regelii

The pectin substances have been isolated fromEremurus regelii Vved., their qualitative and quantitative monosaccharide compositions have been determined, and their physicochemical properties have been studied. The partial hydrolysis of the pectin gave a galacturonan. On the basis of the results of periodate-nitric acid oxidation, enzymatic hydrolysis, and methylation it has been shown that in the galacturoman the galacturonic acid residues are linked by -(1 4)-glycosidic bonds.Deceased.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 172–174, March–April, 1985.     

Box–Behnken Design (BBD)-Based Optimization of Microwave-Assisted Extraction of Parthenolide from the Stems of Tarconanthus camphoratus and Cytotoxic Analysis

Parthenolide, a strong cytotoxic compound found in different parts of Tarchonanthus camphoratus which motivated the authors to develop an optimized microwave-assisted extraction (MEA) method using Box–Behnken design (BBD) for efficient extraction of parthenolide from the stem of T. camphoratus and its validation by high-performance thin-layer chromatography (HPTLC) and cytotoxic analysis. The optimized parameters for microwave extraction were determined as: 51.5 °C extraction temperature, 50.8 min extraction time, and 211 W microwave power. A quadratic polynomial model was found the most suitable model with R² of 0.9989 and coefficient of variation (CV) of 0.2898%. The high values of adjusted R² (0.9974), predicted R² (0.9945), and signal-to-noise ratio (74.23) indicated a good correlation and adequate signal, respectively. HPTLC analyzed the parthenolide (R_f = 0.16) content in T. camphoratus methanol extract (TCME) at λ_max = 575 nm and found it as 0.9273% ± 0.0487% w/w, which was a higher than expected yield (0.9157% w/w). The TCME exhibited good cytotoxicity against HepG2 and MCF-7 cell lines (IC₅₀ = 30.87 and 35.41 µg/mL, respectively), which further supported our findings of high parthenolide content in TCME. This optimized MAE method can be further applied to efficiently extract parthenolide from marketed herbal supplements containing different Tarconanthus species.     

Optimization of Extraction Process and the Antioxidant Activity of Phenolics from Sanghuangporus baumii

Sanghuangporus baumii, is a widely used medicinal fungus. The polyphenols extracted from this fungus exert antioxidant, anti-inflammatory, and hypoglycemic effects. In this study, polyphenols from the fruiting bodies of S. baumii were obtained using the deep eutectic solvent (DES) extraction method. The factors affecting the extraction yield were investigated at different conditions. Based on the results from single-factor experiments, response surface methodology was used to optimize the extraction conditions. The scavenging ability of the polyphenols on •OH, DPPH, and ABTS⁺ was determined. The results showed that the DES system composed of choline chloride and malic acid had the best extraction yield (6.37 mg/g). The optimal extraction parameters for response surface methodology were as follows: 42 min, 58 ℃, 1:34 solid–liquid (mg/mL), and water content of 39%. Under these conditions, the yield of polyphenols was the highest (12.58 mg/g). At 0.30 mg/mL, the scavenging ability of the polyphenols on •OH, DPPH, and ABTS⁺ was 95.71%, 91.08%, and 85.52%, respectively. Thus, the method using DES was more effective than the conventional method of extracting phenolic compounds from the fruiting bodies of S. baumii. Moreover, the extracted polyphenols exhibited potent antioxidant activity.     

Dispersive liquid-liquid microextraction for the isolation and HPLC-DAD determination of three major capsaicinoids in Capsicum annuum L.

Dispersive liquid-liquid microextraction (DLLME) was combined with high-performance liquid chromatography-diode-array detector (HPLC-DAD) for the extraction and quantitation of three major capsaicinoids (i.e. capsaicin, dihydrocapsaicin and nordihydrocapsaicin) from pepper (Capsicum annuum L.). Chloroform (extraction solvent, 100 μL), acetonitrile (disperser solvent, 1250 μL) and 30 s extraction time were found optimum. The analytes were back-extracted into 300 μL of 50 mM sodium hydroxide/ methanol, 45/55% (v/v), within 15 s before being injected into the instrument. Enrichment factors ranged from 3.3 to 14.7 and limits of detection from 5.0 to 15.0 µg g^-1. Coefficients of determination (R²) and %RSD were higher than 0.9962 and lower than 7.5%, respectively. The proposed method was efficiently applied for the extraction and quantitation of the three capsaicinoids in six cultivars of Capsicum annuum L. with percentage relative recoveries in the range of 92.0%–108.0%. DLLME was also scaled up for the isolation of the three major capsaicinoids providing purity greater than 98.0% as confirmed by liquid chromatography-mass spectrometry (LC-MS) and nuclear magnetic resonance (NMR) analysis, which significantly reduced the extraction time and organic solvent consumption.     

Potential of visible-near infrared spectroscopy combined with chemometrics for analysis of some constituents of coffee and banana residues

Banana (stalk, leaf, rhizome, rachis and stem) and coffee (leaf and husks) residues are promising feedstock for fuel and chemical production. In this work we show the potential of near-infrared spectroscopy (NIR) and multivariate analysis to replace reference methods in the characterization of some constituents of coffee and banana residues. The evaluated parameters were Klason lignin (KL), acid soluble lignin (ASL), total lignin (TL), extractives, moisture, ash and acid insoluble residue (AIR) contents of 104 banana residues (B) and102 coffee (C) residues from Brazil. PLS models were built for banana (B), coffee (C) and pooled samples (B + C). The precision of NIR methodology was better (p < 0.05) than the reference method for almost all the parameters, being worse for moisture. With the exception of ash (B and C) and ASL (C) content, which was predicted poorly (R² < 0.80), the models for all the analytes exhibited R² > 0.80. The range error ratios varied from 4.5 to 16.0. Based on the results of external validation, the statistical tests and figures of merit, NIR spectroscopy proved to be useful for chemical prediction of banana and coffee residues and can be used as a faster and more economical alternative to the standard methodologies.     

Chemical investigation of the polysaccharides of the leaves ofPlantago major L.

Summary 1. A polysaccharide has been isolated from the leaves ofPlantage major L. and its monosaccharide composition has been studied.2. It has been established that the polysaccharide investigated contains D-galacturonic acid, D-galactose, D-glucose, D-xylose, L-rhamnose, L-arabinose, a partially methylated galactose, and two unidentified monosaccharides.3. The high content of galacturonic residues (68%) in the polysaccharide enables it to be classified as a pectin.Khimiya Prirodnykh Soedinenii, Vol. 1, No. 5, pp. 297–302, 1965     

Use of modified rice husks as a natural solid adsorbent of trace metals: characterisation and development of an on-line preconcentration system for cadmium and lead determination by FAAS

The use of rice husks as an alternative adsorbent in an on-line preconcentration system for Cd (II) and Pb (II) determination by flame atomic absorption spectrometry (FAAS) is described. The potential of rice husks as a natural adsorbent was evaluated as a material modified with 0.75 mol l⁻¹ NaOH solution and in the unmodified form. For this task, several techniques such as spectroscopy and thermogravimetry were used for elucidation of possible functional groups responsible for the uptake of Cd (II) and Pb (II). Furthermore, based on adsorption studies and adsorption isotherms applied to the Langmüir model, it was possible to verify that modified rice husks present a higher adsorption capacity for both metals. After establishing this material as a promising natural adsorbent, it was used for on-line preconcentration of Cd (II) and Pb (II) metals. The multivariate optimisation of chemical and flow variables was performed by using a full factorial design (2⁴) including the following factors: preconcentration time, preconcentration flow rate, concentration and volume of eluent. The optimum pH values used for on-line preconcentration were taken from prior univariate experiments. Under optimised conditions for Cd (II) determination (4 min of preconcentration at a 6 ml min⁻¹ preconcentration flow rate, in which comprises 24 ml of preconcentration volume, 200 μl elution volume and 1.0 mol l⁻¹ HNO₃ solution as eluent), the system achieved a detection limit of 1.14 μg l⁻¹ and an enrichment factor of 72.4. Similar conditions were used for Pb (II) determination (4 min of preconcentration, 6 ml min⁻¹ preconcentration flow rate, 300 μl elution volume and 1.0 mol l⁻¹ HNO₃ solution as eluent) from which a detection limit of 14.1 μg l⁻¹ and enrichment factor of 46.0 were achieved. Also, rice husks have been shown to be a homogeneous and stable adsorbent in which more than 100 preconcentration/elution cycles provide a relative standard deviation (RSD) of less than 6.0% on the analytical signal. The satisfactory accuracy of the method developed was obtained by using spiked water samples (mineral water and lake water) and spiked red wine samples. These values were confirmed by electrothermal atomic absorption spectrometry (ETAAS). The certified reference material [pig kidney (CRM 186)] and the reference material [beech leaves (CRM 100)] were also used.     

Optimization of polysaccharides extraction from quince peels: partial characterization,antioxidant and antiproliferative properties

Abstract

In this study, Box-Behnken Design was used to optimize the ultrasonic extraction of polysaccharides from quince peels (QPPs) by ascorbic acid and the effect of extraction temperature, extraction time and pH was evaluated. Under optimized conditions of temperature 90?°C, 60?min sonication time and pH?=?3.26, the extraction yield, the galacturonic acid yield and the concentration of sample required to scavenge 50% of 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic) acid (ABTS) values of QPPs were respectively 10.25%, 3.86% and 1.35?mg/mL. The QPPs extracted under optimum conditions was characterized by Fourier transform infrared spectroscopy (FTIR), Nuclear magnetic resonance (^1?H NMR) and Size exclusion chromatography (SEC/MALS/VD/DRI). The monosaccharide analysis revealed that arabinose was the most abundant, followed by galactose, glucose, mannose and xylose. Moreover, QPPs showed significant antioxidant activities (2,2-diphenyl-1-picrylhydrazyl (DPPH) and Ferric- reducing antioxidant power (FRAP)) and reduced viability of human Caco-2 and murine B-16 cell lines in a dose-dependent manner. Hence QPPs could be used as antitumor agent in functional foods andpharmaceutical industries.     

Study on Extraction Process of Root of Henry Wood Betony Polysaccharides and Their Antitumor Activity against S180

We optimized the hot water extraction of polysaccharides from the root of Henry wood betony (RHWPs) using a uniform test and explored their anti-tumor activities in vitro and in vivo. The optimal extraction conditions were as follows: 40 min extraction time, liquid/solid ratio 30 mL/g, 100 min soaking time, two extraction cycles, 100% ethanol concentration, and extraction temperature of 80 °C. The molecular weight distribution of RHWPs with MWs was 228,600 g/mol and 5001 g/mol. The IR spectrum further indicated that RHWPs are acidic polysaccharides containing pyranose and furan rings. The main monosaccharides found in RHWPs were mannose, ribose, l-rhamnose monohydrate, glucuronic acid, galacturonic acid, glucose, galactose, xylose, arabinose, and fucose. RHWPs inhibited the proliferation of S180 tumor cells and induced apoptosis in vitro. Oral administration of RHWPs to tumor-bearing mice significantly inhibited the growth of the S180 xenografts, accelerated apoptosis in tumor cells, and expanded the necrotic regions. Furthermore, RHWPs also markedly increased the levels of TNF-α, IFN-γ, and IL-2 in the sera of tumor-bearing mice, and activated immune cells such as lymphocytes, NK cells, and macrophages, thereby inducing tumor cell apoptosis. Taken together, RHWPs are a promising anti-tumor agent that ought to be explored further.     

Bioactive Components,Volatile Profile and In Vitro Antioxidative Properties of Taxus baccata L. Red Arils

This study aimed at assessing the composition of bioactive compounds, including ascorbic acid, carotenoids and polyphenols, the volatile compound profile and the antioxidant activity of red arils (RAs) of Taxus baccata L. grown in diverse locations in Poland. Among the carotenoids assayed in high quantities (3.3–5.42 μg/g), the lycopene content (2.55–4.1 μg/g) was remarkably higher than that in many cultivated fruits. Samples collected from three sites were distinguished by higher amounts of ascorbic acid (125 mg/100 g, on average) than those found in many cultivated berries. Phenylpropanoids quantitatively dominated among the four groups of phenolic compounds. Chromatographic separation enabled the detection of two phenylpropanoid acids: ferulic and p-coumaric. Irrespectively of the growth site, RAs contained substantial amounts of (-)-epicatechin (1080 μg/100 g, on average). A higher ability to scavenge DPPH^● and ABTS^●+ radicals was found in the hydrophilic fraction of RAs from two sites (Warsaw and Koszalin) compared with the other two sites. The volatile compound profile of RAs was dominated by alcohols, followed by ketones, esters and aldehydes. The presence of some volatiles was exclusively related to the specific growth site, which may be regarded as a valuable indicator. The combination of bioactive and volatile compounds and the fairly good antioxidant potential of RAs render them an attractive source for preparing functional foods.     

Near-infrared diffuse reflectance spectroscopy and neural networks for measuring nutritional parameters in chocolate samples

A rapid and non-destructive method has been developed for the characterization of chocolate samples based on diffuse reflectance near-infrared Fourier transform spectroscopy (DRIFTS) and artificial neural networks (ANNs). This methodology provides a potentially useful alternative to time-consuming chemical methods of analysis. To assess its utility, 36 chocolate samples purchased from the Spanish market were analyzed for the determination of the main nutritional parameters like carbohydrates, fat, proteins, energetic value and cocoa content.Direct triplicate measurements of each sample were carried out by DRIFTS. Cluster hierarchical analysis was used for selecting calibration and validation data sets, resulting in a calibration set comprised of 19 samples and a validation data set of 17 samples. As it is common the presence of non-linear effect in reflectance spectroscopy, ANNs was chosen for data pretreatment. The root-mean-square error of prediction (RMSEP) values obtained for carbohydrates, fat, energetic value and cocoa were 1.0% (w/w), 1.0% (w/w), 50 kJ (100 g)⁻¹ and 1.4%, respectively. The mean difference (d_x-y) and standard deviation of mean differences (s_x-y) of the carbohydrates, fat, proteins content, energetic value and cocoa content were 0.9 and 2.4% (w/w), 0.2 and 1.0% (w/w), 9.1 and 50 kJ (100 g)⁻¹, and −0.5 and 1.4%, respectively. The maximum relative error for the prediction (QC) of any of these parameters for a new sample did not exceed 5.2%.     

Thermal behavior of different cocoa powder varieties and their physicochemical,phytochemical and microbiological characteristics

Four cocoa powder varieties processed in different European countries (Germany, Poland, Romania and Bulgaria) were subjected to physicochemical, phytochemical and microbiological analysis. The cocoa powders were extensively characterized by recording their pH and titratable acidity, respectively, the polyphenols and also the methylxantine derivatives content (theobromine and caffeine). The cocoa powders pH ranged between 5.37 and 8.23, while the titratable acidity was 3.2–4.3 miliequivalent (100 g)^?1 of cocoa powder. Their total polyphenols content ranged between 0.986?÷?2.003 g GAE/(100 g)^?1. The methylxanthine derivatives (theobromine and caffeine) were analyzed by the HPLC method and ranges of 0.992–1.174% for theobromine and 0.096–0.369% for caffeine were obtained. Thermal analysis (TG–DTA) combined with mass spectrometry (MS) elucidated the decomposition processes and the volatile substances (CO, CO₂, H₂O, NO, theobromine, caffeine). The thermal analysis revealed transformations in the cocoa powders composition: drying and water loss; decomposition of pectic polysaccharides; lipids, amino acids and proteins, crystalline phase transformations and carbonizations. The microbiological analysis tested the degree of preservation of the cocoa powders across time, specifically immediately after unwrapping and after 14 days.

     

Supercritical Carbon Dioxide Extraction of Four Medicinal Mediterranean Plants: Investigation of Chemical Composition and Antioxidant Activity

With everyday advances in the field of pharmaceuticals, medicinal plants have high priority regarding the introduction of novel synthetic compounds by the usage of environmentally friendly extraction technologies. Herein, a supercritical CO₂ extraction method was implemented in the analysis of four plants (chamomile, St. John’s wort, yarrow, and curry plant) after which the non-targeted analysis of the chemical composition, phenolic content, and antioxidant activity was evaluated. The extraction yield was the highest for the chamomile (5%), while moderate yields were obtained for the other three plants. The chemical composition analyzed by gas chromatography-high-resolution mass spectrometry (GC-HRMS) and liquid chromatography-high-resolution mass spectrometry (LC-HRMS) demonstrated extraction of diverse compounds including terpenes and terpenoids, fatty acids, flavonoids and coumarins, functionalized phytosterols, and polyphenols. Voltammetry of microfilm immobilized on a glassy carbon electrode using square-wave voltammetry (SWV) was applied in the analysis of extracts. It was found that antioxidant activity obtained by SWV correlates well to 1,1-diphenyl-2-picrylhidrazine (DPPH) radical assay (R² = 0.818) and ferric reducing antioxidant power (FRAP) assay (R² = 0.640), but not to the total phenolic content (R² = 0.092). Effective results were obtained in terms of activity showing the potential usage of supercritical CO2 extraction to acquire bioactive compounds of interest.     

Determination of copper in powdered chocolate samples by slurry-sampling flame atomic-absorption spectrometry

Chocolate is a complex sample with a high content of organic compounds and its analysis generally involves digestion procedures that might include the risk of losses and/or contamination. The determination of copper in chocolate is important because copper compounds are extensively used as fungicides in the farming of cocoa. In this paper, a slurry-sampling flame atomic-absorption spectrometric method is proposed for determination of copper in powdered chocolate samples. Optimization was carried out using univariate methodology involving the variables nature and concentration of the acid solution for slurry preparation, sonication time, and sample mass. The recommended conditions include a sample mass of 0.2 g, 2.0 mol L^–1 hydrochloric acid solution, and a sonication time of 15 min. The calibration curve was prepared using aqueous copper standards in 2.0 mol L^–1 hydrochloric acid. This method allowed determination of copper in chocolate with a detection limit of 0.4 g g^–1 and precision, expressed as relative standard deviation (RSD), of 2.5% (n=10) for a copper content of approximately 30 g g^–1, using a chocolate mass of 0.2 g. The accuracy was confirmed by analyzing the certified reference materials NIST SRM 1568a rice flour and NIES CRM 10-b rice flour. The proposed method was used for determination of copper in three powdered chocolate samples, the copper content of which varied between 26.6 and 31.5 g g^–1. The results showed no significant differences with those obtained after complete digestion, using a t-test for comparison.     

Effect of Extraction Solvent and Temperature on Polyphenol Profiles,Antioxidant and Anti-Inflammatory Effects of Red Grape Skin By-Product

A fully-detailed LC-MS qualitative profiling of red grape skin, extracted with a mixture of ethanol and water (70:30 v:v) has permitted the identification of 65 compounds which can be classified into the following chemical classes: organic and phenolic acids (14 compounds), stilbenoids (1 compound), flavanols (21 compounds), flavonols (15 compounds) and anthocyanins (14 compounds). The extraction yield obtained with water at different temperatures (100 °C, 70 °C, room temperature) was then evaluated and the overall polyphenol content indicates that EtOH:H₂O solvent is the most efficient and selective for polyphenol extraction. However, by analyzing the recovery yield of each single polyphenol, we found that water extraction under heating conditions is effective (extraction yield similar or even better in respect to the binary solvent) for some polyphenolic classes, such as hydrophilic procyanidins, phenolic acids, flavonol glucosides and stilbenoids. However, according to their lipophilic character, a poor yield was found for the most lipophilic components, such as flavonol aglycones, and in general for anthocyanins. The radical scavenging activity was in accordance with the polyphenol content, and hence, much higher for the extract obtained with the binary solvent in respect to water extraction. All the tested extracts were found to have an anti-inflammatory activity in the R3/1 cell line with NF-kb reporter challenged with 0.01 µg/mL of IL-1α, in a 1 to 250 µg/mL concentration range. An intriguing result was that the EtOH:H₂O extract was found to be superimposable with that obtained using water at 100 °C despite the lower polyphenol content. Taken together, the results show the bioactive potentialities of grape skin extracts and the possibility to exploit this rich industrial waste. Water extraction carried out by heating is an easy, low-cost and environmentally friendly extraction method for some polyphenol classes and may have great potential for extracts with anti-inflammatory activities.