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Antioxidants from aqueous decoction of carob pods biomass (Ceretonia siliqua L.): Optimisation using response surface methodology and phenolic profile by capillary electrophoresis
Abstract
Carob (Ceratonia siliqua L.) kibbles, a by-product of the carob bean gum production, were extracted by decoction and evaluated for its phenolic profile and potential use as an added-value antioxidant-rich product. The effect of decoction time (8–20 min) and temperature (80–100 °C) on the polyphenols content and overall antioxidant capacity expressed as percentage inhibition of the DPPH and ABTS free radicals, was performed using a Doehlert experimental design to assess the antioxidants extraction efficiency. It was observed that temperature had the most significant effect. The best conditions for total polyphenols and tannins extraction were 98.5 °C and 17 min, where ca. 39.5 mg GAE/g kibbles and 25.8 mg GAE/g kibbles on a dry basis were obtained, respectively. Under these conditions, inhibition of DPPH and ABTS radicals were 85% and 90%, respectively, showing the promising use of this biomass as an antioxidant source, which could be used, for example, in functional beverages.
... Almanasrah et al. [61] devised a two-step water extraction method to achieve an optimum value of 19.00 mg GAE/g Carob dry matter [61]. This result is lower than that reported by Roseiro et al. [62] for optimized decoction (39.50 mg GAE/g Carob dry matter) and optimized extraction of phenolics from Carob kibbles by Huma et al. [63] who reported 70.11 mg GAE/g dry matter, 68.78 mg GAE/g dry matter, and 69.87 mg GAE/g dry matter using microwave, ultrasound, and conventional solvent, respectively, under the same optimal conditions [62,63].Moreover, Quiles-Carrillo et al. [64] obtained an optimum TPC value of 33.60 mg GAE/g dw by optimized microwave extraction. On the other hand, our results gave higher amounts of TPC compared to the optimum value of TPC of 14.24 mg GAE/g dry Carob matter reported recently by Christou et al. [65]. ...
... Almanasrah et al. [61] devised a two-step water extraction method to achieve an optimum value of 19.00 mg GAE/g Carob dry matter [61]. This result is lower than that reported by Roseiro et al. [62] for optimized decoction (39.50 mg GAE/g Carob dry matter) and optimized extraction of phenolics from Carob kibbles by Huma et al. [63] who reported 70.11 mg GAE/g dry matter, 68.78 mg GAE/g dry matter, and 69.87 mg GAE/g dry matter using microwave, ultrasound, and conventional solvent, respectively, under the same optimal conditions [62,63].Moreover, Quiles-Carrillo et al. [64] obtained an optimum TPC value of 33.60 mg GAE/g dw by optimized microwave extraction. On the other hand, our results gave higher amounts of TPC compared to the optimum value of TPC of 14.24 mg GAE/g dry Carob matter reported recently by Christou et al. [65]. ...
... Independent parameters were selected on the basis of the results of our preliminary assays and of previous research regarding the extraction of phenolic compounds from Carob extracts, which are associated with the plant material antioxidant activity [60,62,63,70,71]. The afore-mentioned researchers suggested that the solvent concentration, the extraction time, and the extraction temperature were the variables with the most influence on the extraction process. ...
Citation: Ayad, R.; Ayad, R.; Bourekoua, H.; Lefahal, M.; Makhloufi, E.H.; Akkal, S.; Medjroubi, K.; Nieto, G. Process Optimization of Phytoantioxidant and Photoprotective Compounds from Carob Pods (Ceratonia siliqua L.) Using Ultrasonic Assisted Extraction Method. Molecules 2022, 27, 8802.
... Almanasrah et al. [61] devised a two-step water extraction method to achieve an optimum value of 19.00 mg GAE/g Carob dry matter [61]. This result is lower than that reported by Roseiro et al. [62] for optimized decoction (39.50 mg GAE/g Carob dry matter) and optimized extraction of phenolics from Carob kibbles by Huma et al. [63] who reported 70.11 mg GAE/g dry matter, 68.78 mg GAE/g dry matter, and 69.87 mg GAE/g dry matter using microwave, ultrasound, and conventional solvent, respectively, under the same optimal conditions [62,63].Moreover, Quiles-Carrillo et al. [64] obtained an optimum TPC value of 33.60 mg GAE/g dw by optimized microwave extraction. On the other hand, our results gave higher amounts of TPC compared to the optimum value of TPC of 14.24 mg GAE/g dry Carob matter reported recently by Christou et al. [65]. ...
... Almanasrah et al. [61] devised a two-step water extraction method to achieve an optimum value of 19.00 mg GAE/g Carob dry matter [61]. This result is lower than that reported by Roseiro et al. [62] for optimized decoction (39.50 mg GAE/g Carob dry matter) and optimized extraction of phenolics from Carob kibbles by Huma et al. [63] who reported 70.11 mg GAE/g dry matter, 68.78 mg GAE/g dry matter, and 69.87 mg GAE/g dry matter using microwave, ultrasound, and conventional solvent, respectively, under the same optimal conditions [62,63].Moreover, Quiles-Carrillo et al. [64] obtained an optimum TPC value of 33.60 mg GAE/g dw by optimized microwave extraction. On the other hand, our results gave higher amounts of TPC compared to the optimum value of TPC of 14.24 mg GAE/g dry Carob matter reported recently by Christou et al. [65]. ...
... Independent parameters were selected on the basis of the results of our preliminary assays and of previous research regarding the extraction of phenolic compounds from Carob extracts, which are associated with the plant material antioxidant activity [60,62,63,70,71]. The afore-mentioned researchers suggested that the solvent concentration, the extraction time, and the extraction temperature were the variables with the most influence on the extraction process. ...
The current study first describes the extraction of phytoantioxidant polyphenols from Carob byproducts (pods) using maceration and heating-assisted extraction as traditional methods and ultrasonic-assisted extraction (UAE) as an innovative method to determine the most efficient extraction process in terms of four targeted responses: total phenolic content (TPC), antioxidant activities (TAC and DPPH), and photoprotective properties as measured by the sun protection factor (SPF). Second, we used response surface methodology (RSM) with a central composite rotatable design (CCDR) approach to investigate the influence of process variables (extraction time, extraction temperature, and solvent concentration) on UAE, which was found to be the most effective extraction technique in our study. Carob byproduct extracts had a TPC ranging from 6.21 to 21.92 mg GAE/g dw, a TAC ranging from 22.00 to 49.30 mg AAE/g dw, DPPH scavenging activity ranging from 56.35 to 90.50%, and SPF values ranging from 8.62 to 22.37. The optimal UAE conditions for maximum TPC, TAC, DPPH, and SPF responses were determined to be 38.90% ethanol, 53.90 °C, and 50.92 min. Using Carob as a source for sustainable and bioactive products in conjunction with optimized UAE is a promising contribution to the cosmetic industry that will help to strengthen the concept of environmentally-friendly “green chemistry”. Given that Carob pulp or seeds are considered food byproducts, the research presented here encourages the use of these agri-food waste materials in cosmetics.
... Almanasrah et al. [61] devised a two-step water extraction method to achieve an optimum value of 19.00 mg GAE/g Carob dry matter [61]. This result is lower than that reported by Roseiro et al. [62] for optimized decoction (39.50 mg GAE/g Carob dry matter) and optimized extraction of phenolics from Carob kibbles by Huma et al. [63] who reported 70.11 mg GAE/g dry matter, 68.78 mg GAE/g dry matter, and 69.87 mg GAE/g dry matter using microwave, ultrasound, and conventional solvent, respectively, under the same optimal conditions [62,63].Moreover, Quiles-Carrillo et al. [64] obtained an optimum TPC value of 33.60 mg GAE/g dw by optimized microwave extraction. On the other hand, our results gave higher amounts of TPC compared to the optimum value of TPC of 14.24 mg GAE/g dry Carob matter reported recently by Christou et al. [65]. ...
... Almanasrah et al. [61] devised a two-step water extraction method to achieve an optimum value of 19.00 mg GAE/g Carob dry matter [61]. This result is lower than that reported by Roseiro et al. [62] for optimized decoction (39.50 mg GAE/g Carob dry matter) and optimized extraction of phenolics from Carob kibbles by Huma et al. [63] who reported 70.11 mg GAE/g dry matter, 68.78 mg GAE/g dry matter, and 69.87 mg GAE/g dry matter using microwave, ultrasound, and conventional solvent, respectively, under the same optimal conditions [62,63].Moreover, Quiles-Carrillo et al. [64] obtained an optimum TPC value of 33.60 mg GAE/g dw by optimized microwave extraction. On the other hand, our results gave higher amounts of TPC compared to the optimum value of TPC of 14.24 mg GAE/g dry Carob matter reported recently by Christou et al. [65]. ...
... Independent parameters were selected on the basis of the results of our preliminary assays and of previous research regarding the extraction of phenolic compounds from Carob extracts, which are associated with the plant material antioxidant activity [60,62,63,70,71]. The afore-mentioned researchers suggested that the solvent concentration, the extraction time, and the extraction temperature were the variables with the most influence on the extraction process. ...
The current study first describes the extraction of phytoantioxidant polyphenols from Carob byproducts (pods) using maceration and heating-assisted extraction as traditional methods and ultrasonic-assisted extraction (UAE) as an innovative method to determine the most efficient extraction process in terms of four targeted responses: total phenolic content (TPC), antioxidant activities (TAC and DPPH), and photoprotective properties as measured by the sun protection factor (SPF). Second, we used response surface methodology (RSM) with a central composite rotatable design (CCDR) approach to investigate the influence of process variables (extraction time, extraction temperature, and solvent concentration) on UAE, which was found to be the most effective extraction technique in our study. Carob byproduct extracts had a TPC ranging from 6.21 to 21.92 mg GAE/g dw, a TAC ranging from 22.00 to 49.30 mg AAE/g dw, DPPH scavenging activity ranging from 56.35 to 90.50%, and SPF values ranging from 8.62 to 22.37. The optimal UAE conditions for maximum TPC, TAC, DPPH, and SPF responses were determined to be 38.90% ethanol, 53.90 °C, and 50.92 min. Using Carob as a source for sustainable and bioactive products in conjunction with optimized UAE is a promising contribution to the cosmetic industry that will help to strengthen the concept of environmentally-friendly “green chemistry”. Given that Carob pulp or seeds are considered food byproducts, the research presented here encourages the use of these agri-food waste materials in cosmetics.
... Total phenolic compounds in hydrolysates and washing solutions (ethanol-water solutions) were determined using the Folin-Ciocalteu colorimetric method according to an improved procedure described elsewhere [25] and adapted to a microplate format using spectrophotometric detection and microtiter 96-well plates. Absorbance was measured at 725 nm in a UV-Vis spectrophotometer (Thermo Scientific™ Multiskan™ GO Microplate Spectrophotometer, Waltham, MA, USA) after 40 min incubation in the dark at room temperature. ...
... Qualitative characterization of the phenolic profile was carried out using capillary zone electrophoresis (CZE) according to a method described before [25] using an Agilent Technologies CE equipment (Waldbronn, Germany) with a DAD detector. A fused-silica uncoated and extended light-path capillary from Agilent with an i.d. ...
... Thus, lignin from agro-forest residues could originate value-added compounds with recognised biological activities (mainly antioxidant, but also antitumoral, antiviral, and immunopotentiation activities, as well as antibacterial and antiparasitic actions [25]) under specific pre-treatment conditions. Tricin from the WS in particular is a flavone with a wide spectrum of health-promoting effects, and is considered one of the most potent anticancer agents tested, most probably due to the stability of its structure, since it was previously detected undegraded in the faeces of tricin-fed rats [36]. ...
Organosolv pre-treatments aiming to selectively remove and depolymerise lignin and hemicellulose and yield an easily digestible cellulose fraction are one of the potential options for industrial implementation within the biorefinery concept. However, the use of high temperatures and/or high catalyst concentrations is still hindering its wide adoption. In this work, mild temperature organosolv processes (140 °C) that were either non-catalysed or catalysed with sulphuric or acetic acid were compared to standard similar conditions using ethanol-based organosolv for both wheat straw (WS) and eucalyptus wood residues (ERs) as agricultural and forestry-derived model raw materials, respectively. The experimental results demonstrated that high cellulose purities could be obtained for the catalysed ethanol-based processing of the WS, which resulted in high saccharification yields (>80%), conversely to the non-catalysed process, which only reached values close to 70%. For eucalyptus residues (ERs), the pulp yields obtained were lower than the values obtained for the WS, suggesting that the ERs were a more reactive material. Cellulose purity was higher than that obtained for the corresponding treatment for the WS, with the highest cellulose purity being obtained for the ethanol-based process catalysed with sulphuric acid. Both materials presented high lignin yield recovery in the liquid stream.
... The determination of PVPP (polyvinylpolypyrrolidone) precipitable phenolic compounds was performed by their adsorption on the insoluble PVPP matrix. The experimental procedure was carried out according to Roseiro et al. (2013). Briefly, 100 mg of PVPP, 1 mL of acidified distilled water (pH 3) and 1 mL of organosolv liquor were added to Eppendorf tubes. ...
... The liquors obtained from the organosolv treatment were analysed for their phenolic profile using a capillary electrophoresis system (Agilent Technologies, Waldbronn, Germany) equipped with a diode array detector, according to the methodology described in Roseiro et al. (2013). Detection was performed at 320 nm and compounds were identified by comparison with UV spectra and migration times of phenolic standards analysed under the same conditions as liquors. ...
... The antioxidant activity of the liquors was expressed as Trolox equivalents (TE) and described by the DPPH percentage inhibition, determined as reported before (Roseiro et al., 2013). ...
Olive stones (OS) constitute a waste lignocellulosic material produced by the olive oil industry in great amounts, that currently is only used as a low-value energy source for industrial or domestic boilers. Having in view its full valorization, this work proposes and validates an integrated strategy aiming to obtain three different streams of sugars / lignin-derived compounds. Dilute acid hydrolysis was used to obtain a xylose-rich hydroysate that was chemically converted into furfural with a 48.7 % yield. The resulting acid-pretreated solid biomass that consisted mainly of lignin and cellulose, was subjected to a catalyzed ethanol-based organosolv delignification. Temperature, time, and sulphuric acid concentration were optimized in order to recover added-value lignin products and digestible cellulose.
At the optimal conditions (190 ᵒC and 30 min), a 50 % delignification was reached, together with the highest enzymatic hydrolysis yields (190 g glucose/kg of OS). Phenolic compounds content in organosolv liquors reached 41.6 mg GAE/g OS. This extract presented an antioxidant capacity up to 10.9 mg TE/g OS. The pretreated solid fraction was used as a substrate for ethanol production by a pre-saccharification and simultaneous saccharification and fermentation process, enabling to obtain an ethanol concentration of 47 g/L, with a fermentation yield of 61.4 % of the theoretical maximum. Globally, from 100 kg of OS processed according to this experimental scheme, 6.9 kg of furfural, 6.2 kg of ethanol, 7.4 kg of lignin, and 4.2 kg of phenolics compounds can be obtained as main products, thus constituting a way of valorization of renewable material in a multiproduct biorefinery strategy.
... Among them, the spectrophotometric methods represent the easiest way to estimate the total phenolic content as well as the antioxidant activity of the samples. In particular, 2,2-diphenyl-1-picrylhydrazyl (DPPH), Ferric Reducing Antioxidant Power (FRAP), 2,2 -azino-bis(3ethylbenzothiazoline-6-sulfonic acid (ABTS), and Oxygen Radical Absorbance Capacity (ORAC) assays have been previously reported in the literature to determine the antioxidant activity of carob samples [9,14,[16][17][18][19]. Since antioxidant activity is directly related to phenolic content, the determination of antioxidant activity is usually followed by the determination of total phenolics, with the Folin-Ciocalteu assay being the most commonly used spectrophotometric method for the estimation of the total phenolic content in carob and its derived products [8,14,[20][21][22]. ...
... The antioxidant capacity of the carob pulp and carob products was determined using the DPPH method, as previously described by Roseiro et al. [18]. The increased DPPH radical scavenging activity is indicated by the decrease in absorbance of the DPPH solution. ...
In recent years, carob and its derived products have gained wide attention due to their health-promoting effects, which are mainly attributed to their phenolic compounds. Carob samples (carob pulps, powders, and syrups) were analyzed to investigate their phenolic profile using high-performance liquid chromatography (HPLC), with gallic acid and rutin being the most abundant compounds. Moreover, the antioxidant capacity and total phenolic content of the samples were estimated through DPPH (IC50 98.83–488.47 mg extract/mL), FRAP (48.58–144.32 μmol TE/g product), and Folin–Ciocalteu (7.20–23.18 mg GAE/g product) spectrophotometric assays. The effect of thermal treatment and geographical origin of carobs and carob-derived products on their phenolic composition was assessed. Both factors significantly affect the concentrations of secondary metabolites and, therefore, samples’ antioxidant activity (p-value < 10−7). The obtained results (antioxidant activity and phenolic profile) were evaluated via chemometrics, through a preliminary principal component analysis (PCA) and orthogonal partial least square-discriminant analysis (OPLS-DA). The OPLS-DA model performed satisfactorily, differentiating all samples according to their matrix. Our results indicate that polyphenols and antioxidant capacity can be chemical markers for the classification of carob and its derived products.
... Various in vitro studies have shown that extracts of the carob tree have a potent antioxidant effect (Roseiro, Tavares, Roseiro, & Rauter, 2013;Sebai et al., 2013). They also have strong scavenging activity on reactive oxygen and free radicals, thus reducing oxidative damage (Roseiro, Duarte, et al., 2013;Roseiro, Tavares, et al., 2013). ...
... Various in vitro studies have shown that extracts of the carob tree have a potent antioxidant effect (Roseiro, Tavares, Roseiro, & Rauter, 2013;Sebai et al., 2013). They also have strong scavenging activity on reactive oxygen and free radicals, thus reducing oxidative damage (Roseiro, Duarte, et al., 2013;Roseiro, Tavares, et al., 2013). ...
Macerates of kibbles, seeds and leaves of Ceratonia siliqua L. were prepared and analysed to apply them for the development of a new multilayer active packaging. The profile of forty-three different bioactive volatile compounds was obtained employing headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). The antioxidant capacity was investigated using the following methods: 2,2-diphenyl-1-picrylhydrazyl and phosphomolybdenum method, which demonstrated stronger antioxidant capacity in the case of seeds macerates. However, the analysis of the antimicrobial properties of the different macerates versus Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli revealed a weak antibacterial activity. Additionally, the different macerates were incorporated into an adhesive used to build a new biopackaging multilayer film based on cellulose polymer, whose antioxidant capacity was evaluated by two different methods (2,2-diphenyl-1-picrylhydrazyl and hydroxyl radical assay). The films with the best antioxidant activity, containing carob seeds macerates, were selected for the food safety assessment through migration assay. The obtained results showed no migrants, neither in the case of the volatile compounds nor non-volatile ones. Besides, the CIE L*a*b* colour of the active films was evaluated. The obtained results are therefore promising for future production of active biopackaging at an industrial scale.
... As it has been proven, the efficiency and effectiveness of employed extraction techniques strongly influence the obtained polyphenolic patterns and compositions of carob extracts. Various conventional extraction methods including maceration, infusion, decoction, and Soxhlet extraction have, so far, been utilized for the recovery of polyphenols from carob pods and derived products [6][7][8][9]. However, these classical techniques are often time-consuming, they require relatively large quantities of solvents, and the examined active components may degrade or oxidise due to the long processing times and high temperatures used [4,10]. ...
... In addition, despite its extensive use in phytochemicals analysis, capillary electrophoresis (CE) has not been previously applied for both the qualitative and quantitative determination of carob pulp phenolics. Although and attempted to analyse carob pulp phenolics by use of a CE system, they failed to achieve a complete separation, identification and quantification of the target analytes [7,22,23]. ...
Polyphenols in carobs have recently attracted great attention due to their wide range of biological and health promoting effects. A comprehensive study was conducted to find an optimum method for the extraction, purification and characterization of these valuable bioactive substances. Under this framework, the ultrasound-assisted extraction (UAE) of polyphenols from carob pulp was optimized by the maximization of the yield in total phenolics using response surface methodology. In particular, the effects of solid-solvent ratio, solvent concentration, extraction time, sonication amplitude, and sonication mode were investigated and optimized using a complete experimental design. In comparison to conventional extraction techniques, UAE offered a higher yield of antioxidants and a shorter processing time. Solid-phase extraction was evaluated as a clean-up strategy prior to the electrophoretic analysis of extracts. The results from the analysis of real samples revealed the predominance of gallic acid and highlighted the great influence of the ripening stage on carobs composition.
... Acquiring data in this manner provided information on both intact precursor ions and fragment ions simultaneously. Data were acquired and processed using The radical scavenging ability of the extracts was measured from the bleaching of the purple-colored methanolic solution of DPPH following the procedure described by Roseiro et al. [25]. Briefly, extract solutions were appropriately diluted (25 mg sample mL −1 ) and mixed with 975 µL of freshly prepared DPPH methanolic solution (60 µM) or extraction solvent (blank). ...
Colocasia esculenta L. leaves are considered a by-product of taro cultivation and are discarded as environmental waste, despite their valuable phenolic composition. Their valorization to obtain value-added substances for medicinal, food, and cosmetic applications is the aim of the current work. An ultrasound-assisted extraction was developed for the environmentally friendly and sustainable isolation of taro leaf antioxidants using natural deep eutectic solvents (NaDESs). Among the utilized solvents, the NaDES based on betaine and ethylene glycol provided the best extraction efficiencies in terms of polyphenolic content and antioxidant activity. Multi-response optimization suggested a solvent-to-solid ratio of 10 mL g−1, a processing time of 60 min, an extraction temperature of 60 °C, and a water content of 33.8% (w/w) as optimal extraction parameters. Leaf extract obtained under these optimum operational parameters demonstrated a strong radical scavenging activity against 2,2-diphenyl-1-picrylhydrazyl (65.80 ± 0.87%), a high ferric reducing antioxidant power (126.62 ± 1.92 μmol TE g−1 sample), and significant protection against oxidative stress-induced DNA damage. The chromatographic characterization of the optimum extract revealed its richness in flavonoids (flavones and flavonols). The outcomes of the present study suggest that the proposed method could serve as a highly efficient and green alternative for the recovery of polyphenols from agricultural wastes.
... Therefore, a lot of research has been performed in order to determine and characterize the content of polyphenols in carob pulp flour [8][9][10] and their health impact [11]. Gallic acid was found to be the dominant compound in carob flour extracts, followed by (-)-epigallocatechin, (-)-epigallocatechin gallate and (-)-epicatechin gallate [12]. However, the concentration of total polyphenols in carob flour strongly depends on genetics, the environment and the extraction method [13]. ...
To examine antioxidant capacity and the hepatoprotective effect of carob pulp flour, microwave-assisted extraction was performed. The influence of ethanol concentration (0–40% w/w), extraction time (5–25 min) and irradiation power (400–800 W) on DPPH, FRAP and ABTS antioxidant activity of carob pulp flour extract was evaluated. The strongest influence was that of the ethanol concentration, followed by extraction time. Optimal process parameters for maximizing total antioxidant activity were determined, using response surface methodology: ethanol concentration 40%, time 25 min and power 800 W. Carob extract obtained at optimal conditions (CE) was analyzed in vivo using a paracetamol-induced hepatotoxicity model in mice. Treatment with CE attenuated the parameters of liver injury, especially aspartate and alanine aminotransferase activity, and prevented paracetamol-induced increase in malondialdehyde levels. Pretreatment with CE reversed the activities of superoxide dismutase, catalase, glutathione peroxidase and glutathione S-transferase enzymes after the high dose of paracetamol in the liver. Hepatotoxicity induced using a toxic dose of paracetamol was also seen through histopathological alterations, which were significantly reduced in the groups treated with CE prior to paracetamol. Still, the number of Kupffer cells and macrophages did not differ among groups. Finally, pretreatment of mice with CE and paracetamol significantly decreased the expression of cytochrome P450 2E1 (CYP2E1) in hepatocytes.
... This method is based on the spectrophotometric measurement of NADH formed through the combined action of D-lactate dehydrogenase (D-LDH) and D-alanine aminotransferase (D-ALT/D-GPT). The total amount of phenolics was determined by the Folin-Ciocalteu colourimetric method using a microplate spectrophotometer (Multi-skanTM GO, Thermo Scientific, USA) adapted by Roseiro et al. (2013) and detailed in Alves-Ferreira et al. (2019b) using gallic acid as standard. Cell growth was evaluated by measuring the optical density at 600 nm using a spectrophotometer (Helios Alpha, Thermo Scientific, USA). ...
In this study, glucan-rich solids, and xylose-rich hydrolysates obtained from Cistus ladanifer distillery residues (CLR) were used for d-lactic acid (d-LA) production by the d-lactogenic Escherichia coli strain JU15. Firstly, hemicellulosic hydrolysates obtained by the autohydrolysis process were submitted to dilute sulfuric acid-catalysed post-hydrolysis. The influence of operational conditions on oligosaccharides hydrolysis was assessed by the combined severity parameter (CS) in the range of 1.1–2.3. The optimum post-hydrolysis conditions were found for CS of 1.6 (300 mM H2SO4, 15 min, 121 °C). Subsequent detoxification procedures on post hydrolysed liquors were carried out, where 9.1% (w/v) powdered activated charcoal enabled a full removal of furfural, 5-hydroxymethylfurfural (HMF), and phenolic compounds together with a reduction of acetic acid (37%), and formic acid (27%). Diverse fermentation modes using detoxified and non-detoxified hydrolysates, as well as using previously NaOH delignified glucan-rich solids alone (SHF or SSF) or together with pentoses liquors (SSCF) (5% loading) were performed. For all the tested conditions, both hemicellulose- and cellulose-derived sugars can be efficiently used as the carbon source to produce d-lactic acid by E. coli JU15 with a d-LA yield always surpassing 92 gd-LA/100 g sugars.
... These concentrations were the highest determined in this work; higher than those determined with 50% acetone or 50% ethanol, especially in the case of flavonoids (1.5-fold higher; Table 2). These results compare favourably with those reported for the aqueous extraction of carob pod biomass at 98 • C and 3% solids [61], eucalyptus wood at 50 • C and 10% biomass for 90 min [51], or brewer's spent grains at 80 • C and 5% solids [62]. ...
Exhausted olive pomace (EOP) is a residue derived from the olive pomace oil industry. One of the main components of this agro-industrial residue is the extractive fraction which contains non-structural components such as bioactive compounds. In this work, different extraction methods, including green technologies, have been compared to evaluate the extraction of antioxidants from EOP: hydrothermal extraction, aqueous accelerated extraction, organosolv extraction, and extraction with aqueous salt solutions. The extracts obtained were characterized regarding the content of total phenols by the Folin–Ciocalteu method. After characterization, hydroxytyrosol was found to be one of the potential active compounds in EOP.
... The antioxidant activity of the extracts revealed to be in accordance with the TPC, being the results higher for UAE extracts, particularly, using water-acetone. These values are higher than those reported for carob kibbles using UAE [14]; 9.4 mg GAE/g dry mass for water and 20.4 mg GAE/g dry mass for 70% acetone. They were also higher than those for brewer's spent grains using maceration [15], 3.6 mg GAE/g dry mass for water, and 9.90 mg GAE/g dry mass for 60% acetone. ...
The exhausted olive pomace (EOP) is the main residue generated year-round after the extraction of the residual oil contained in the olive pomace. Due to its chemical composition, EOP is an interesting bioresource for the production of bioenergy and high added-value products. Therefore, the purpose of this study was to evaluate the extraction of antioxidants from EOP using sequential ultrasound-assisted extraction (UAE) and maceration with constant stirring. Water and 70% acetone were used as solvents. The total phenolic content was determined by the Folin–Ciocalteu method, the antioxidant capacity was investigated and the phenolic extracts were also characterized.
... ; Bachir bey,Meziant, Benchikh, & Louaileche, 2014;Belwal, Dhyani, Bhatt, Rawal, & Pande, 2016;Benito-Román, Alvarez, Alonso, Cocero, & Saldaña, 2015;Campos, Chirinos, Barreto, Noratto, & Pedreschi, 2013;El Ksibi, Slama, Faidi, & Ticha, 2015;Fernández, Espino, Gomez, & Silva, 2018;Grosso et al., 2014;Pompeu, Silva, & Rogez, 2009;Roseiro, Tavares, Roseiro, & Rauter, 2013;Saikia, Mahnot, & Mahanta, 2015;Wang et al., 2013;Wani et al., 2017), MAE(Bouras et al., 2015;Dahmoune et al., 2014Dahmoune et al., , 2015Elez Garofulić et al., 2013;Li et al., 2012;Mellouk et al., 2016;Nayak et al., 2015;Setyaningsih et al., 2015;Song, Li, Liu, & Zhang, 2011; Wu et al., 2012), UAE (; ; ; ; ; ;Chen et al., 2015Chen et al., , 2018Fang et al., 2014;Goldsmith, Vuong, Stathopoulos, Roach, & Scarlett, 2018;González-Centeno et al., 2014;Hani, Torkamani, Zainul Abidin, Mahmood, & Juliano, 2017;Katsampa, Valsamedou, Grigorakis, & Makris, 2015;Nipornram, Tochampa, Rattanatraiwong, & Singanusong, 2018;Pandey, Belwal, Sekar, Bhatt, & Rawal, 2018;Pooralhossini, Ghaedi, Zanjanchi, & Asfaram, 2017;Ş ahin & Ş amlı, 2013;Sharmila et al., 2016) and various other methods such as supercritical fluid extraction, cold extraction, super critical CO 2 extraction and semi continuous hot-cold Extraction(Monrad, Srinivas, Howard, & King, 2012;Pinela et al., 2018;Valadez-Carmona, Ortiz- Moreno, Ceballos-Reyes, Mendiola, & Ibáñez, 2018). All of the abovementioned methods have been optimized by using RSM employing ...
Phenolic compounds from plant sources have significant health-promoting properties and are known to be an integral part of folk and herbal medicines. Consumption of phenolics is known to alleviate the risk of various lifestyle diseases including cancer, cardiovascular, diabetes, and Alzheimer’s. In this context, numerous plant crops have been explored and characterized based on phenolic compounds for their use as supplements, nutraceutical, and pharmaceuticals. The present review highlights some important source of bioactive phenolic compounds and novel technologies for their efficient extraction. These techniques include the use of microwave, ultrasound, and supercritical methods. Besides, the review will also highlight the use of response surface methodology (RSM) as a statistical tool for optimizing the recoveries of the phenolic bioactives from plant-based matrices.
... The antioxidant activity was expressed in TEAC (Trolox Equivalent Antioxidant Capacity). The decreasing of the DPPH solution absorbance indicated an increase of the DPPH radical-scavenging activity [34]. Analytical measures of described parameters were performed at the beginning (IN) and at the end (OUT) of the assay experimental time. ...
Olive oil and pig productions are important industries in Portugal that generate large volumes of wastewater with high organic load and toxicity, raising environmental concerns. The principal objective of this study is to energetically valorize these organic effluents—piggery effluent and olive mill wastewater—through the anaerobic digestion to the biogas/methane production, by means of the effluent complementarity concept. Several mixtures of piggery effluent were tested, with an increasing percentage of olive mill wastewater. The best performance was obtained for samples of piggery effluent alone and in admixture with 30% of OMW, which provided the same volume of biogas (0.8 L, 70% CH4), 63/75% COD removal, and 434/489 L CH4/kg SVin, respectively. The validation of the process was assessed by molecular evaluation through Next Generation Sequencing (NGS) of the 16S rRNA gene. The structure of the microbial communities for both samples, throughout the anaerobic process, was characterized by the predominance of bacterial populations belonging to the phylum Firmicutes, mainly Clostridiales, with Bacteroidetes being the subdominant populations. Archaea populations belonging to the genus Methanosarcina became predominant throughout anaerobic digestion, confirming the formation of methane mainly from acetate, in line with the greatest removal of volatile fatty acids (VFAs) in these samples.
... These concentrations were the highest determined in this work; higher than those determined with 50% acetone or 50% ethanol, especially in the case of flavonoids (1.5-fold higher; Table 2). These results compare favourably with those reported for the aqueous extraction of carob pod biomass at 98 • C and 3% solids [61], eucalyptus wood at 50 • C and 10% biomass for 90 min [51], or brewer's spent grains at 80 • C and 5% solids [62]. ...
Exhausted olive pomace (EOP) is the waste generated from the drying and subsequent extraction of residual oil from the olive pomace. In this work, the effect of different aqueous solvents on the recovery of antioxidant compounds from this lignocellulosic biomass was assessed. Water extraction was selected as the best option for recovering bioactive compounds from EOP, and the influence of the main operational parameters involved in the extraction was evaluated by response surface methodology. Aqueous extraction of EOP under optimised conditions (10% solids, 85 ºC, and 90 min) yielded an extract with concentrations (per g EOP) of phenolic compounds and flavonoids of 44.5 mg gallic acid equivalent and 114.9 mg rutin equivalent, respectively. Hydroxytyrosol was identified as the major phenolic compound in EOP aqueous extracts. Moreover, these extracts showed high antioxidant activity, as well as moderate bactericidal action against some food-borne pathogens. In general, these results indicate the great potential of EOP as a source of bioactive compounds, with potential uses in several industrial applications.
... Carob pulp is rich in total sugar content (31-50%) that can easily be water extracted to be used for syrups production (El Batal et al. 2011). It can also be exploited for the production of bioethanol (Mazaheri et al. 2012) and natural antioxidants (Roseiro et al. 2013;Benchikh et al. 2014;Amessis-Ouchemoukh et al. 2017). Due to these economical and ecological benefits, many countries have promoted the cultivation and exploitation of this valuable genetic resource (Battle and Tous 1997;Lozzi et al. 2015). ...
La présente invention fourni un nouveau milieu nutritif, développé pour la première fois pour la micropropagation in vitro de caroubier. Le milieu nutritif développé contient les éléments essentiels pour la croissance des vitroplants de caroubier àdes concentrations appropriées à cette espèce. La présente invention fourni également un procédé simple, rapide et économique pour la micropropagation de caroubier en utilisant le milieu de culture liquide et la technique d'enracinement ex vitro. Ce procédé constitue un outil important qui pourra faciliter la multiplication en masse de vitroplants de qualité chez le caroubier afin de répondre à la demande mondiale croissante en matière de cette espèce.
... Carob (Ceratonia siliqua L.) is a perennial leguminous, an evergreen plant widely grown in the Mediterranean region with great economic and environmental potential where it covers hills and large mountain areas of the arid and the semi-arid regions [17,18]. World production of carob is about 422,334 tons per year [19], where the pods consist of 90% pulp and 10% seeds by weight [20]. It is utilized as a raw material in different food industries including animal feed, cakes and yogurt production [21,22]. ...
Lignocellulosic biomass from agricultural residues is a promising feedstock for lactic acid (LA) production. The aim of the current study was to investigate the production of LA from different lignocellulosic biomass. The LA production from banana peduncles using strain Bacillus coagulans with yeast extract resulted in 26.6 g LA·L−1, and yield of 0.90 g LA·g−1 sugars. The sugarcane fermentation with yeast extract resulted in 46.5 g LA·L−1, and yield of 0.88 g LA·g−1 sugars. Carob showed that addition of yeast extract resulted in higher productivity of 3.2 g LA·L−1·h−1 compared to without yeast extract where1.95 g LA·L−1·h−1 was obtained. Interestingly, similar LA production was obtained by the end where 54.8 and 51.4 g·L−1 were obtained with and without yeast extract, respectively. A pilot scale of 35 L using carob biomass fermentation without yeast extract resulted in yield of 0.84 g LA·g−1 sugars, and productivity of 2.30 g LA·L−1·h−1 which indicate a very promising process for future industrial production of LA.
... In the last decade, there have been some attempts to recover phenolic antioxidants from carob fruit using different extraction techniques and solvents [9][10][11]. In addition, researchers have attempted to utilize carob antioxidants to reduce lipid oxidation in cooked pork meat [12], Atlantic horse mackerel [13], and sunflower [14] as well as improve the antioxidant potential in durum wheat pasta [15] and milk beverages [16]. ...
The goal of this study was to explore the potential of carob extracts to act as lipid inhibitors in model food systems. First, the extraction efficacy of fourteen solvents on the phenolic and flavonoid contents as well as on the antioxidant activity was assessed. Results showed that the phenolic composition and antioxidant activity of the extracts were strongly affected by solvents. Subsequently, the antioxidant potential of the most promising extracts (water, methanol, acidic acetone, and acetone–water) against four model food systems were evaluated. The acidic acetone extract had the highest antioxidant activity (70.3 ± 5.3%) in the β-carotene-linoleic acid system, followed by the acetone–water extract (62.1 ± 4.9%). Both extracts significantly prevented the lipid oxidation in sunflower oil and cooked comminuted pork; the inhibition activity at the end of storage period was 36.7–50.5% and 17.4–24.8%, respectively. A reduction of 49.5–54.8% in the formation of dienes in the oil-in-water emulsion was also found. The inhibitory effect of methanolic and aqueous extracts was significantly lower. Qualitative and quantitative variations in extracts are responsible for this antioxidant behavior in food systems. Gallic acid, myrecetin, rutin, and catechin are the main components of the extracts while myricetin and quercetin play an essential role in the antioxidant activity, according to the biochromatograms.
... Carob pulp is rich in total sugar content (31-50%) that can easily be water extracted to be used for syrups production (El Batal et al. 2011). It can also be exploited for the production of bioethanol (Mazaheri et al. 2012) and natural antioxidants (Roseiro et al. 2013;Benchikh et al. 2014;Amessis-Ouchemoukh et al. 2017). Due to these economical and ecological benefits, many countries have promoted the cultivation and exploitation of this valuable genetic resource (Battle and Tous 1997;Lozzi et al. 2015). ...
A new basal culture medium was developed and tested using a rapid and efficient protocol of in vitro axillary shoot bud proliferation of Ceratonia siliqua L., an important Mediterranean Fabaceae plant species. In a first experiment, the new formulated ‘LA’ mineral composition significantly improved shoot growth and proliferation as compared with Murashige and Skoog medium (MS, 1962) in both solid and liquid culture media. However, the liquid culture system proved to be the most suitable for shoot induction, shoot length (about fourfold higher), and multiplication rate (about two-fold higher), the difference being significant. The measured growth and proliferation parameters were further improved when LA mineral composition was optimized, in a second experiment. The highest multiplication rate (6.3) was achieved during the second subculture using the optimized ‘LAC’ medium. Noticeably, hyperhydricity and shoot-tip necrosis symptoms were absent in both formulated LA and LAC compositions when using the liquid culture system. In vitro rooting in solid medium showed 41.7 to 46.3% response on a solid medium which was more suitable than the liquid culture system, the difference being significant. In contrast, pretreated microcuttings with 3 μM IBA (indole-3-butyric acid) were successfully rooted ex vitro, showing significantly higher response (91.7%), average root number (8.3), and root length (31.5 mm). The plantlets were successfully acclimatized showing more than 90% survivability and normal morphology. The present study is a first cost-effective protocol for carob micropropagation combining the use of the newly formulated LAC basal medium, a liquid culture system, and ex vitro rooting.
... Diphenyl-picryl hydrazide (DPPH) and 2,2 -azino-bis-(3-ethyl-benzthiazoline-6-sulphonate) (ABTS + ) are two common free radicals often used for evaluating antioxidant capacity of samples. One paper in 2012 [47] showed that DPPH and ABTS + were employed in measuring the overall antioxidant capacity of Carob kibbles, a by-product of the carob bean gum production, followed by phenolic profile analysis using CE. Another paper employed CE to separate the extract of tomato skin and identify the antioxidants, including phenolics and flavonoids, after off-line reaction of DPPH and the sample [48]. ...
Bioactive ingredients of natural products can protect human body from harm, as well as prevent and treat disease. Screening bioactive compounds from natural products is attracting particular attention. It is a great challenge to separate and detect the active compounds from complex matrix natural products. Capillary electrophoresis (CE) plays a vital role in screening active compounds because of its unique features such as high-efficiency separation, short analysis time, minimal sample consumption and ease to realize automatization etc. Additionally, CE has been developed various modes owing to its abundant advantages in analysis and separation of compounds. The purpose of this work is to review previous developments and applications of CE in screening bioactive compounds derived from natural products from 2007 to 2017. This review does not only summarize the traditional methods of detecting active ingredients but also briefly introduces some novel assays. The trends in the application of CE in active compounds screening are addressed in the article.
Liposome capillary electrokinetic chromatography was used to investigate the interactions between three β-blockers of different hydrophobicity and various liposome solutions. The studied β-blockers comprised alprenolol, propranolol, and carvedilol. The composition of the liposome solutions, containing 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine, 1,2-dioleoyl-sn-glycero-3-phos-phoethanolamine, 1-palmitoyl-2-oleoyl-sn-glycero-3-phospho-l-serine, and cholesterol in various molar ratios, was designed by a response surface methodology-central composite design approach. Subsequently, after conducting the liposome capillary electrokinetic chromatography experiments and determining the retention factors from the electrophoretic mobilities of the compounds, and further calculating the distribution coefficients, an analysis of variance was performed. After extracting the statistical models, optimal operational conditions were obtained based on the developed models. To further investigate the interactions between the β-blockers and the liposomes, nanoplasmonic sensing experiments were carried out on two different liposome systems. The overall results demonstrate the strong influence of cholesterol and 1-palmitoyl-2-oleoyl-sn-glycero-3-phospho-l-serine on the distribution coefficients.
The carob tree is a common tree throughout the world. It has received great attention due to its potent biological effects and diverse industrial applications resulting from its richness in phytochemicals, particularly polyphenols. The polyphenol content, the phenolic composition, and the antioxidant activity of carob were studied with variable results. Several factors are involved in this variability, such as gender, variety, cultivar, ripening stage, environmental conditions, and extraction techniques. Also, the bioaccessibility of carob polyphenols is strongly affected by several factors, such as the phenolic fraction, food matrix, structure of compounds, and particle size. As a result, the purpose of this paper is to discuss the various factors of variation as well as the extraction and encapsulation techniques used to improve their recovery and bioaccessibility.
This reference describes recent advances and applications of capillary electrophoresis in the field of food science. The first two chapters are devoted to the fundamentals of capillary electrophoresis, and to the main sample preparation techniques used for food analysis using this miniaturized separation technique, respectively. These two introductory chapters are followed by several chapters focused on the different strategies for analyzing specific food components, including lipids, carbohydrates, proteins, peptides, amino acids, vitamins, polyphenols, and food additives.
The information provided in these chapters helps readers to understand and develop appropriate methods to carry out a deep characterization of food samples. Relevant concepts such as food authentication, chemical food safety or the control of the quality and safety of dietary supplements, and food metabolomics are also covered, where appropriate. The big potential of capillary electrophoresis to achieve chiral separations and the determination of enantiomers in food samples or to develop targeted and non-targeted metabolomics strategies to ensure food safety and quality is also described. As an additional step towards analytical miniaturization, a chapter devoted to food analysis by microchip electrophoresis is also included in this book. All 14 chapters are contributed by highly experienced researchers in the field.
Capillary Electrophoresis in Food Analysis is a key source of information for food chemists and analytical chemists in industry (quality control laboratories) and academia (research labs and training courses).
Hippophae rhamnoides L. polysaccharide was optimized with flash extraction by response surface design. The optimum process conditions were: rotation rate 5000 r/min, extraction time 15 s, extraction temperature 90 ℃ and liquid‐to‐material ratio 38 mL/g, the extraction yield was 15.28±0.02%. HRP‐1 and HRP‐2 obtained by 40% and 60% graded alcohol precipitation were characterized. The results indicated that HRP‐1 and HRP‐2 both composed of mannose, ribose, rhamnose, glucuronic acid, galacturonic acid, glucose, galactose, xylose, arabinose with different molar ratio and the molecular weights were 380.59 kDa and 288.24 kDa, respectively. In addition, the in vitro antioxidant and immunoenhancement activities of HRP‐1 and HRP‐2 were analyzed, and the two fractions showed good free radical scavenging activity against ·OH, ABTS·+, DPPH·, and extremely strong immunomodulatory activity against RAW264.7 cells. Indicating that flash extraction is suitable with HRP, the structural study of HRP provides a scientific theoretical basis for the development of Hippophae rhamnoides.
Carob has been used by humans since antiquity. Its major use is food, but traditional medicines
of many nations used it for treatments of various health disorders. The fruits (pods or kibbles)
were the main source for nutrition and medicinal uses, but decoctions and extracts were prepared
from other parts of the tree, especially leaves. Modern science has analyzed most of the chemical
compositions of the different parts, and among the phytochemicals that were found, antioxidants
play very important roles in Carob nutritional and medicinal activities. So, in addition to having strong
antioxidant activity and due to it, these natural products, their extracts, and foods that contain them,
have anticancer, neuroprotective, hepatoprotective, antiaging, skin care, antidiabetic, and others.
Phenolics and carbohydrates are the strongest antioxidants, but some volatile compounds have
the same activity, to some extent. However, this review will present Carob antioxidants, their major
nutritional and medicinal activities, and suggest future horizons for their use in human wellbeing.
The carob (Ceratonia siliqua L.), a plant that grows widely in the Mediterranean climate, has a very dry and hard fruit that contains substantial amounts of sugar and phenolic compounds. This study aimed to determine the optimum extraction conditions for obtaining pure sugar extract with the least undesired compounds from the dried carob pod, and exclude the phenolic compounds that contribute to bitterness, astringency, turbidity, and color. In this study, the effect of extraction parameters as the fruit particle size (X1: 0.30–3.67 mm or 50.0–5.0 mesh), water: fruit ratio (liquid/solid ratio, X2: 2.3–5.7 ml g-1), extraction temperature (X3: 15–75 °C), and extraction time (X4: 44–196 min) on sugar composition and phenolic contents of carob extract was evaluated and an experimental design was developed using response surface methodology central composite design. When the effects of the interactions between the factors on the sugar concentration of carob extract were examined; the most significant effect (p<0.01) was shown by the extraction temperature and extraction time interaction (X3 × X4). The interactions of particle size and water: fruit ratio (X1 × X2) and interactions of particle size and extraction time (X1 × X4) were statistically significant (p<0.05). The optimum extraction conditions were determined as X1: 4.0 mm (5.0 mesh), X2: 4 ml g–1, X3: 20 °C, and X4: 200 minutes. In this study, the individual effects of the factors (X1, X2, X3, and X4) on the extraction were examined and the interaction effects of factors on responses to the extract. Consequently, regression equations showed the relations between the responses and the tested factors.
Brewery wastewater (BWW) is an appealing low-cost substrate for the production of single cell oils by oleaginous microorganisms. However, it may contain inhibitor compounds that may affect the microbial metabolism. This work investigated, for the first time, the presence of potential inhibitor compounds in primary brewery wastewater (PBWW) and secondary brewery wastewater (SBWW) for the pure and mixed cultivation of the yeast Rhodosporidium toruloides NCYC 921 and the microalga Tetradesmus obliquus ACOI 204/07. Three organic acids (OrgAc) were identified in the brewery effluents (acetic, propionic and butyric acids). Yeast and microalga pure and mixed cultivations were performed in PBWW and SBWW in order to understand the behaviour of the microorganisms, individually and together. Flow cytometry (FC) was used to monitor each microbial population during the mixed cultivations, and to study the yeast and microalga cell viability throughout all cultivations. The yeast cells in pure cultures grown in both effluents were severely affected by the OrgAc presence confirmed by the cell stress results obtained by FC. However, in the mixed cultures, the yeast cells were able to develop, and the levels of stress conditions were considerably lower. Only in microalga pure and mixed cultures efficient OrgAc removal was observed.
Polyphenols with high chemical diversity are present in vegetables both in the edible parts and by-products. A large proportion of them remains unabsorbed along the gastrointestinal tract, being accumulated in the colon, where they are metabolized by the intestinal microbiota. These polyphenols have been found to have "prebiotic-like" effects. The edible plant industry generates tons of residues called by-products, which consist of unutilized plant tissues (peels, husks, calyxes and seeds). Their disposal requires special and costly treatments to avoid environmental complications. Reintroducing these by-products into the value chain using technological and biotechnological practices is highly appealing since many of them contain nutrients and bioactive compounds, such as polyphenols, with many health-promoting properties. Edible plant by-products as a source of polyphenols highlights the need for analytical methods. Analytical methods are becoming increasingly selective, sensitive and precise, but the great breakthrough lies in the pretreatment of the sample and in particular in the extraction methods. This review shows the importance of edible plant by-products as a source of polyphenols, due to their prebiotic effect, and to compile the most appropriate analytical methods for the determination of the total content of phenolic compounds as well as the detection and quantification of individual polyphenols.
In the current study, an eco‑friendly management technology to improve young carob (Ceratonia siliqua L.) tree tolerance to water deficit was set up by using single or combined treatments of arbuscular mycorrhizal fungi (AMF) and/or compost (C). Two groups of young carob have been installed: (i) carob cultivated under well‑watered conditions (WW; 70% field capacity (FC)) and (ii) where the plants were drought‑stressed (DS; 35% FC) during 2, 4, 6, and 8 months. The effect of used biofertilizers on the course of growth, physiological (photosynthetic traits, water status, osmolytes, and mineral content), and biochemical (hydrogen peroxide (H2O2), oxidative damage to lipids
(malondialdehyde (MDA), and membrane stability (MS)) traits in response to short‑ and long‑term droughts were assessed. The dual application of AMF and C (C + AMF) boosted growth, physiological and biochemical parameters, and nutrient uptake in carob under WW and DS. After eight months, C + AMF significantly enhanced stomatal conductance by 20%, maximum photochemical efficiency of PSII by 7%, leaf water potential by 23%, chlorophyll and carotenoid by 40%, plant uptake of mineral nutrients (P by 75%, N by 46%, K+ by 35%, and Ca2+ by 40%), concentrations of soluble sugar by
40%, and protein content by 44% than controls under DS conditions. Notably, C + AMF reduced the accumulation of H2O2 and MDA content to a greater degree and increased MS. In contrast, enzyme activities (superoxide dismutase, catalase, peroxidase, and polyphenoloxidase) significantly increased in C + AMF plants under DS. Overall, our findings suggest that the pairing of C + AMF can mediate superior drought tolerance in young carob trees by increasing leaf stomatal conductance, cellular water content, higher solute concentration, and defense response against oxidative damage during the prolonged period of DS.
In this work, a simple, reliable, and fast capillary electrophoretic method was developed and validated for the simultaneous determination of 12 polyphenolic compounds, the most frequently found in carob's pulp and seeds. The present work deals with the development of a novel dual electrophoretic system based on the combined use of β‐CD and ionic liquid (IL) as buffer additives. A baseline separation of the target analytes was achieved in less than 10 min by using a BGE consisting of 35 mM borate along with 15 mM β‐CD and 3 mM L‐alanine tert butyl ester lactate (L‐AlaC4Lac) IL as buffer additives at pH 9.5, a temperature of 25°C and an applied voltage of 30 kV. The application of the developed electrophoretic method to real samples enabled the identification and quantification of the main phenolic constituents of both ripe and unripe carob pulp extracts. The results revealed the predominance of gallic acid in both ripe (183.92 μg/g carob pulp) and unripe (205.10 μg/g carob pulp) carob pulp and highlighted the great influence of the ripening stage on carobs polyphenolic composition, with unripe pods being more enriched in polyphenols (total phenolics detected: 912.58 and 283.13 μg/g unripe and ripe carob pulp). This article is protected by copyright. All rights reserved
Obtaining high-quality value-added bread with extended shelf-life by utilizing food industry by-products that would have minimal negative effect on gluten structure while avoiding the usage of synthetic preservatives, was the challenge of this study. For this purpose the influence of the combination of carob pod flour (C, 0–15%), sugar beet fibers (F, 0–10%) and sugar beet molasses (M, 0–6%) on dough rheology and bread quality was investigated. Selected materials were of good microbiological quality, while carob flour and sugar beet fibers were rich in dietary fibers (43.6% and 67.0%, respectively). The presence of high share of dietary fibers (combination of C and F) increased dough resistance to extension up to 2.5 times, while dough extensibility was reduced by 50%. The addition of molasses had less pronounced single effect on dough properties however its impact in combination with fiber-rich materials outweighed the individual effect (an increase of dough resistance at about 55%). Molasses alone and in combination with other ingredients had positive effect on bread quality. Sample M6F5 attained crumb quality score (6.0 of maximum 7.0) higher than in control sample (5.6). High share of C and F reduced loaf volume and crumb quality of bread up to 56% and 50%, respectively and increased hardness 7.5 times. However, carob flour (7.5%) increased polyphenols content and antioxidant capacity 3 and 4 times, respectively. Moreover, carob flour and molasses and their combination showed inhibitory effect on mold mycelia growth and spores formation. Regarding all of the above, C7.5M3F5 was chosen as optimal sample.
The yeast Rhodosporidium toruloides NCYC 921 was used for lipid production, using Miscanthus biomass hydrolysate as carbon source. The hydrolysate was obtained by enzymatic hydrolysis of Miscanthus biomass (at high solids loading) previously subjected to a hydrothermal pre-treatment. Afterwards R. toruloides was grown on Miscanthus sp. hydrolysate (MH), undiluted and diluted, at the ratios of 1:4 (20% v/v), 1:2 (33.3% v/v) and 3:1 (75% v/v). The best yeast performance was observed for MH 1:2 medium dilution, reaching the maximal biomass concentration of 6.3 g/L, the lipid content of 30.67% w/w dry cell weight and the lipid concentration of 1.64 g/L. Flow cytometry demonstrated that R. toruloides cell membrane was massively damaged when the yeast was grown on undiluted MH, due to the presence of phenolic compounds; however, when the yeast was grown on diluted MH 1:2 and 1:4, the proportion of intact cells has increased during the yeast cultivation.
Decoction extraction procedure was implemented to regain phenolic compounds from C. citratus leaves. The extraction variables, solid/liquid ratio (2–5 g/100 mL), temperature (85–95 °C), and time (5–10 min) were assessed by central composite design for process optimization. Antioxidant activity (DPPH) and total polyphenol content (TPC) were monitored as responses. The TPC and DPPH were 71.98 ± 0.33 mg GAE/100 mL extract and 80.63 ± 0.49 mg TE/100mL extract respectively under optimal conditions (solid/liquid ratio = 5, temperature = 93.8 °C and time 11.3 min). The evaluation of phenolic compounds and volatile compounds of C. citratus extract at conditions for optimum extraction revealed that caffeic (20.81 ± 0.003 mg/100mL) and syringic acids (18.63 ± 7.390 mg/100mL) were the main phenolic compounds while citral and geraniol were the primary volatile compounds. The results achieved herein suits the potential use of C. citratus extract as natural source of antioxidant and aroma compounds that can be employed in different industrial sectors.
Practical application
Lemongrass obtained at the optimal extraction conditions is a good source of antioxidants and the extract has organic acids and a lemon scent due to the presence of citral. This extract can thereby be incorporated in the production of beverages which can help aromatize the beverage and also contribute in the addition of the antioxidant property of the beverage. It is also rich in organic acids, the main being propionic acid, which is known to have antimicrobial activity primarily against bacteria and mold. The lemongrass extract can therefore, extend the shelf life of the beverage they are incorporated in and also the citral present in lemongrass has antimicrobial properties.
Background
Non‐diary beverages with probiotic properties are of a great interest nowadays. In this research, we evaluated the suitability of carob kibbles in the manufacture of kvass. Kvass is a low alcoholic drink popular in Central and Eastern Europe and indicated as a potential non‐diary beverage with probiotic properties. Therefore, the viability of probiotic strains of L. plantarum and S. boulardii during 4‐week storage in manufactured beverages was also tested.
Results
Carob kibbles introduced significant amounts of phenolic compounds to kvasses, especially gallic acid (up to 117.45 ± 10.56 mg/L) and improved antiradical activity up to 78% after fermentation. Moreover, fermentation efficiently reduced furfural and HMF contents in samples up to 12.9 and 29.9%, respectively. Kvasses with rye malt extract possessed coffee‐like, chocolate‐like, roasted and caramel odours and more bitter taste. Whereas kvass with carob kibbles was characterized by fruit‐like odour and sweeter taste. Fermentation contributed to a creation as well as degradation of volatiles. L. plantarum exhibited higher general mortality during storage while, in case of S. boulardii, the viability was significantly higher regardless the sample composition.
Conclusion
This is the first study reporting the use of carob kibbles for kvass production. The obtained results showed that carob kibbles can replace rye malt extract, at least partially, in the production of kvass, giving to the product added health benefits. Moreover, S. boulardii is a better choice for a production of kvass with probiotic properties.
This article is protected by copyright. All rights reserved.
Obtaining essential oils and hydrolates from underutilized biomass is an economic and sustainable way for production of these high added-value bioproducts. However, this process still generates large amounts of residues as the by-products obtained during distillation, which can be a concern for the environment, but also adequate substrates for other applications. Considering this fact, the waste distilled by-products remaining after steam-distillation of underutilized biomass from Cupressus lusitanica and Cistus ladanifer, were evaluated as a natural source of other high value products with biological activities, namely, phenolic compounds. Thus, the remaining extracted solid residues (ESRs) were characterized and subject to further treatments by ultrasound-assisted extraction (UAE) with ethanol and 70 % acetone, in order to prepare phenolic-rich extracts thereof: ESRs(EtOH) and ESRs(70 % Ace). Together with the distiller condensation waters (DCWs), these extracts were characterized for their phenolic content (total phenols, tannins and flavonoids). Their antioxidant activity was also evaluated by different methodologies. The phenolic profile of DCWs, ESRs(EtOH) and ESRs(70 % Ace) from both waste species was obtained by capillary zone electrophoresis (CZE) and phenolic compounds were tentatively identified. Results obtained for C. lusitanica biomass are here disclosed for the first time. Generally, all samples revealed to be rich in phenolic compounds, being C. ladanifer biomass the one with higher phenolic content. DCWs presented values of 140 mgGAE/g for C. lusitanica and 210 mg GAE/g for C. ladanifer, from which ca. 60 % were tannins. Extracts obtained with 70 % acetone were the ones with the highest results, except for the antioxidant activity by xanthine oxidase and superoxide inhibition, which was higher in DCWs. Catechins were the major compounds found for both species, but gallocatechins and gallic acid were only identified in C. ladanifer. Hydroxycinnamic acid derivatives and salicylic acid were also identified in C. ladanifer, partly justifying the anti-inflammatory effect referred for this species.
The main aim of this study was to maximize tartaric acid recovery, and to optimize total phenolics, sugars, and antioxidant activity present in industrial red and white tartar wastes. Total tartaric acid contents were determined at 4.87 and 3.98 g/100g-dry mass of red and white tartar wastes using ion chromatography. Based on chemical precipitation and separation process, tartaric acid crystals were recovered at 4.482 and 3.574 g-TA/100g-dry mass of red and white tartar wastes respectively. Optimum values for solid wastes extraction including pH, temperature, contact time, and solid to solvent ratio were first investigated and determined at 2.0, 45 °C, 30 min, and 1:6 (w/v) for red and white tartar wastes respectively. It was found that aqueous phase of the red and white tartar suspensions contained 0.179 and 0.177 g l−1, 2.31 and 2.51 g l−1, and 64.29 and 53.59 %, whereas solid red and white tartar wastes extracted with ethanol contained 2.549 and 1.058 g l−1, 17.361 and 20.101 g l−1, 90.927 and 62.219 % of total phenolics, sugars, and antioxidant activity respectively. It was investigated that ethanol is the best solvent to extract the total phenolics, sugars, and antioxidant activity in comparison to water, methanol, and ethyl acetate from solid wastes. The overall results showed that red and white tartar wastes could be a good low-cost tartaric acid, phenolics, sugars, and antioxidants sources.
Implementation of green chemistry and biorefinery concept are needed to boost production of biomass-derived fuels, chemicals, and materials with cost-effective processing of sustainable feedstock. The use of imidazole as a novel solvent for biomass pretreatment creates an approach that helps accomplish this concept. The present work is dedicated to study the pretreatment of residual lignocellulosic biomass, namely, extracted solid waste of Cupressus lusitanica, by application of the alkaline solvent—imidazole. The pretreatment allowed obtaining cellulose- and hemicellulose-rich fractions, whereas lignin was depolymerized. Both cellulose and hemicellulose recovery were highly dependent on the reaction conditions. The highest cellulose content was obtained at 160 °C for 4 h and was 40.7 ± 0.6 wt% with a delignification yield of 65.2 ± 0.4 wt%. The effect of biomass delignification on the efficiency of enzymatic digestibility was also analyzed and it was observed a good linear relationship between the delignification yield and the glucan to glucose yield. The presence of added-value phenolic compounds from depolymerized lignin in recovered imidazole was analyzed by capillary electrophoresis and determination of total phenolic content and antioxidant activity was also performed. These compounds were tentatively identified and their structures proposed on the basis of the HPLC–MS analyzes.
Graphic Abstract
Ceratonia siliqua (Carob); is a Mediterranean legume globally recognized for its commercial value, being used as a cold beverage, in bakery and confectionary products. It is widely used as a Cocoa substitute not only due to its richness in sugar but rather the absence of caffeine and theobromine stimulant action. Both fruit pulp and seeds are of potential nutritive and medicinal values. The pulp comprises a high sugar content dominantly sucrose as well as polyphenols viz. phenolic acids, flavonoids and tannins. Seeds potential usage is attributed to its locust bean gum (LBG), commercially and pharmaceutically used as gelling and stiffening agent. Carob syrup is a traditional product native to the Mediterranean region, enriched in D-pinitol sugar of anti-diabetic effect. Considering the diversity of carob active constituents’ classes, a myriad of biological effects is recorded to include antioxidant, anticancer, antimicrobial and anti-hyperlipidemic effects. This book chapter presents up to date information on carob usage and chemistry while providing insight on research questions or applications yet to be addressed.
A microwave-assisted extraction (MAE) procedure to obtain phenolic compounds from carob bark was optimized by using response surface methodology. A four-factor, three-level Box–Behnken design with five central points was used to evaluate the influence of temperature, solid-liquid ratio, ethanol concentration, and time in carob bark extraction in terms of antioxidant activity (DPPH) and total extraction yield. Optimal extraction conditions were found using 80 °C, 35% (v/v) ethanol, a ratio of 35 mL/g, and 29.5 min. Total phenolics content (TPC), antioxidant activity (DPPH, FRAP, ABTS), carbohydrate content, and main polyphenols composition (HPLC) were determined at optimal conditions. An experimental total yield of 66.5% was obtained with a TPC value of 33.6 mg GAE/g DW and polysaccharides content of 345.4 mg glucose/g DW. A high antioxidant activity was also shown by the three methods tested. The results showed the potential of carob pods skin as a natural source of phenolic compounds, in particular gallic acid, and the effectiveness of MAE as extraction technique for the revalorization of this agro-food waste.
The carob is a dome-shaped evergreen tree that is a member of the pea family (Fabaceae). Its fruit has been used for human consumption and as animal feed in the Mediterranean countries for centuries and was also widely used as a herbal remedy in traditional folk’s medicine. In this paper, an in-depth literature review was conducted about this species discussing its history, origins, main current uses, components (both nutrient and bioactive), biological activities, and potential applications as the source of sustainable ingredients and products. Among the many bioactive compounds that were found in carob, the most well studied are polyphenols. The levels of these compounds were found to vary depending on many factors, such as the variety, plant part, geographic location, roasting and extraction conditions, and even analysis methods. In the light of these researches, it was recognized that carob offers several biological activities including antioxidant, anticancer, and anti-diabetic due to the presence of a high quantity of pinitol and antibacterial. Rich in sugars, proteins, and minerals, the carob has a vast range of industrial applications such as cacao substitute, sugars substitute, free from gluten making it cereal-derived foods for celiac people.
Cistus ladanifer residues obtained after essential oil distillation were extracted with ethanol and water (CLRext) and subsequently hydrothermally treated (autohydrolysis) in order to selectively hydrolyze hemicelluloses. The extraction removed a significant amount of potentially valuable compounds (40% w/w, dry basis), foremost, phenolic compounds (0.363 and 0.250 g gallic acid equivalent/g extract, respectively, for water and ethanol). Autohydrolysis was studied under diverse severity factors (log Ro), in the temperature range of 150 to 230 °C. The hydrolyzates mainly contain oligosaccharides, reaching the highest concentration (23.5 g/L) for log Ro of 3.07 (190 °C), corresponding to a yield of 15 g oligosaccharides/100 g dry feedstock. The processed solids are enriched in glucan and lignin. The maximum glucan content (35%) was attained at log Ro of 3.51 (205 °C). Py-GC/MS confirmed the reduction of pentose-derived carbohydrates in the solid after hydrothermal treatment and an increase of syringil units in the lignin compared to the untreated biomass. These results show the potential use of this C. ladanifer residue for the production of phenolic extracts, and hemicellulosic oligosaccharides, together with the production of a cellulose- and lignin-rich solid stream.
The direct liquefaction of the wastes from carob pod processing industry leaded to a biooil with 88% of conversion, further water extraction afforded two extracts that can be used, e.g., as alternatives to the synthetic antioxidants. The hydroxyl number, as well as acid value, were screened for the reaction crude and both extracts. The organic extract, despite its high concentration of phenolic compounds (19.3 g GA eq/mg extrc), proved to be less antioxidant (1.05 μL/mL) than the aqueous congener (total phenolic content, 0.92 GA eq/mg extrc; antioxidant activity, 1.19 μL/mL). Nevertheless, both extracts have proved to be more active than BHT. The composition of the aqueous extract regarding its sugar's content was also studied, revealing the presence of glucose, fructose, and sucrose. The higher heating value, estimated by Dulong’s formula, along with the analysis of van Krevelen diagram indicate that the organic extract can be potentially used as a fuel, an additive or as components in fuel blends. Briefly, this work proves that carob waste can be valued as an antioxidant additive, as fuels or even as a sugar platform.
Background:
The decoction of Pelargonium graveolens yields an antioxidant-rich extract and a water-soluble polysaccharide. This study aims (1) to investigate the effect of process parameters (extraction time and temperature) on the antioxidant activity of the decoction and the extraction yield of CPGP by response methodology and (2) to study the chemical properties of the optimized decoction and rheological properties of the corresponding extracted polysaccharide.
Results:
The antioxidant-rich decoction contained about 19.76 ± 0.41 mg RE/g DM of flavonoids and 5.31 ± 0.56 mg CE/gDM of condensed tannins. The crude Pelargonium graveolens polysaccharide (CPGP) contained 87.27 % of sugar. Furthermore, the CPGP solutions (0.5%, 1%, and 2%) exhibited shear-thinning or pseudoplastic flow behavior. A central composite design (CDD) was applied to assess the effects of temperature and time on the antioxidant activity of the decoction, on the one hand, and on water-soluble polysaccharide yield, on the other. The decoction optimization of Pelargonium graveolens aimed to use less energy (93°C for 11 minutes) leading to the highest values of decoction phenolic content (33.01 ±0.49 mg GAE/gDM) and DPPH scavenging activity (136.10 ± 0.62 mg TXE/gDM) and the highest values of CPGP yield (6.97%).
Conclusion:
The obtained results suggest that the CPGP rheological characteristics are suitable for applications in many industries, especially food. The values of optimal conditions showed that Pelargonium graveolens decoction operation could have multiple uses, especially for consuming less energy.
Carob tree ( Ceratonia siliqua L.) is one of the most widespread medicinal plants in the Mediterranean area. Traditionally, it was cultivated for its ethnopharmacological benefits and, more especially, for the seeds, which served as unit of measurement of jewelers “carat.” Hence, in the last half-century, numerous studies reported a wide range of phytoconstituents contained in all parts of Ceratonia siliqua such as phenolic compounds, flavonoids, tannins, anthocyanins, alkaloids, glycosides, proteins and minerals. This review article unveils the phytochemical constituents, bioactivity and pharmacological studies of Ceratonia siliqua . Recent studies have shown that the extracts of this plant exhibit an antioxidant, antidiarrheal, antibacterial, antifungal, anti-inflammatory, antidiabetic activities and also hepatoprotective and antiproliferative effects. In this review, we provide a summary of the most interesting data related to bioactivity and therapeutic potential of Ceratonia siliqua in a way to suggest possible future studies that may use Ceratonia siliqua as an undeniable natural alternative for neurodegenerative diseases treatment.
Grapes (Vitis vinifera) are produced in large amounts worldwide and mostly are used for winemaking. Their untreated wastes are rich in valuable secondary metabolites, such as phenolics. Thus, in this study, white and red wine wastes (“Malagouzia” and “Syrah” variety) were investigated for their added value phenolics, which were analyzed by HPLC-ESI/MS and subsequently encapsulated in several polymers. Extracts from all wastes gave high amounts of total phenolics (13±2.72-22±2.69 mg g⁻¹) and possessed high antioxidant activity (67-97%). In addition to their significant antibacterial activity against gram-negative and gram-positive bacteria, interesting results were also obtained from their anti-inflammatory and antiplatelet activity, in vitro. Encapsulation of the extracts was selective, leaving out most of sugars and other organic compounds when alginate-chitosan were used. Encapsulation efficiency recorded for all extracts ranged from 55 to 79%. Release studies were also performed in several solutions aiming in their commercial use in food and pharmaceutical industries.
Purpose: The aim of this study was to optimize hydrothermal treatments (autohydrolysis) for selective hydrolysis of hemicelluloses in the residues obtained from the industrial steam distillation of Cistus ladanifer (rock-rose) for essential oil extraction (CLR). The effect of the autohydrolysis in the removal of extractives of these residues was also evaluated. Methods: The raw material was treated with water in a 6:1 liquid-to-solid ratio (w/w) and the effect of temperature (130–230 °C) on the composition of liquid and solid phases were evaluated and interpreted using the severity factor (log R0). Results: The highest recovery of oligosaccharides (24.7 g/L), corresponding to a yield of 28.4 g/100 g of CLR was obtained at moderate conditions, log R0 of 3.12. Together with hemicelluloses, polar extracts were also largely solubilized during the hydrothermal process yielding hydrolysates with a relevant concentration of phenolics. The highest glucan content (35.6 g/100 g of CLR) of the solid residue was obtained at more severe conditions, log R0 of 4.0 (220 °C). There was no apparent lignin solubilisation in any of the conditions, which is an advantage of this hydrolytic pretreatment. Conclusions: Cistus ladanifer residues demonstrated to have potential to be used in the biorefinery framework with a full upgrade of all biomass fractions. © 2017 Springer Science+Business Media B.V., part of Springer Nature
The main objective of this research was to compare physicochemical parameters, antioxidant activity, lipid composition, and sensory analysis of initial and roasted carob pod powder ( Ceratonia siliqua L.) obtained at different roasting temperatures. The roasted products became darker and the average moisture content, water activity, oil content, and sweetness values decreased at higher temperatures. Total polyphenol content and antioxidant activity increased with increasing roasted temperature. Oleic acid, linoleic acid, and palmitic acid were the main fatty acids present in carob oil. Results showed that the roasted carob pod powders are sweeter, have more caramel-like taste, and have more cacao-like aroma at lower roasting temperatures but have more astringent taste, coffee-like aroma, and roasted aroma at higher roasting temperatures.
In an experiment with 32 male growing Florina (Pelagonia) lambs, effects of replacing barley grain, sunflower meal and wheat bran with partly destoned exhausted olive cake (PDEOC) and soybean meal on productivity, carcass characteristics, meat chemical composition and meat fatty acid (FA) composition was determined. In the 56. day experiment, lambs were randomly allocated into four dietary treatments (PDEOC0, PDEOC80, PDEOC160, and PDEOC240) of 8 lambs each and accommodated in individual floor pens. Lambs had an initial body weight (BW) of 16.7. ±. 1.81. kg, and were fed one of four isonitrogenous (crude protein 162. g/kg, dry matter - DM basis) and isoenergetic (net energy for gain 6.11. MJ/kg, DM basis) concentrate mixtures ad libitum and alfalfa hay (0.2. kg DM/lamb/day). The PDEOC was added to the concentrate mixture at inclusion levels (as mixed basis) of 0, 80, 160, and 240. kg/t for treatments PDEOC0, PDEOC80, PDEOC160, and PDEOC240, respectively. No differences (P. >. 0.05) occurred among PDEOC treatments in final BW (29.9. kg), BW gain (0.24. kg/day), DM intake (0.97. kg/day), and feed conversion ratio (4.07. kg DM intake/kg BW gain). Moreover, meat chemical composition and carcass characteristics were not affected (P. >. 0.05) with increased PDEOC feeding, except for the fat color, fat firmness, wetness and overall acceptability of carcasses that linearly increased with increasing PDEOC supplementation. Oleic and palmitic acids were the predominant FA in intramuscular fat of all treatments. FA were not affected (P. >. 0.05) with increased PDEOC feeding, except for the lauric acid which decreased (P = 0.018), as well as the α-linolenic acid which increased (P = 0.020). PDEOC supplementation, at levels up to 240. kg/t of concentrate mixtures, in isonitrogenous and iso (net energy) energetic diets for growing lambs did not affect their performance and carcass characteristics, while it improved carcass qualitative traits.
Total mass transfer coefficients of soluble solids (SS) and total phenolic compounds (TPC) were determined during carob extraction. The Arrhenius equation was applied to determine the efficiency of process temperature, as an alternative approach to Fick's second law. Carob pod, cut into small pieces (internal diameter: 5–7 mm), was contacted with water in batch system to extract SS by continuous circulation of water at different temperatures (20, 50 and 85C). The process was also performed at 85C using an industrial-scale extractor. Activation energies for both SS and TPC diffusions were calculated as 5.84 and 0.072 × 10−3 kJ/mol, respectively. As expected, higher extract concentrations were achieved with higher temperatures. In contrast, high extraction temperature, even at 85C, did not cause hydroxymethylfurfural (HMF) formation. As the increase in temperature does not affect formation of HMF during carob pod extraction, higher operational temperatures such as 80–90C may be applied to obtain higher solute concentrations.
The possibility of utilising chopped and deseeded carob pods (kibbles) as a source of polyphenolic antioxidants was examined by performing extractions with various solvent systems, in order to evaluate and optimize the conditions for the recovery of polyphenols. Maximum quantities of polyphenolic components were found in 80 % acetone extracts, as evaluated by measuring total polyphenol and total flavanol content. By contrast, ethyl ace-tate was inefficient in extracting polyphenols. The assessment of the antioxidant potency of carob pod extracts employing two characteristic in vitro models showed that carobs con-tain polyphenols with appreciable antiradical and reducing properties. The values obtained were compared to the data on red wines and pure polyphenolic antioxidants.
A method for the screening of antioxidant activity is reported as a decolorization assay applicable to both lipophilic and hydrophilic antioxidants, including flavonoids, hydroxycinnamates, carotenoids, and plasma antioxidants. The pre-formed radical monocation of 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS*+) is generated by oxidation of ABTS with potassium persulfate and is reduced in the presence of such hydrogen-donating antioxidants. The influences of both the concentration of antioxidant and duration of reaction on the inhibition of the radical cation absorption are taken into account when determining the antioxidant activity. This assay clearly improves the original TEAC assay (the ferryl myoglobin/ABTS assay) for the determination of antioxidant activity in a number of ways. First, the chemistry involves the direct generation of the ABTS radical monocation with no involvement of an intermediary radical. Second, it is a decolorization assay; thus the radical cation is pre-formed prior to addition of antioxidant test systems, rather than the generation of the radical taking place continually in the presence of the antioxidant. Hence the results obtained with the improved system may not always be directly comparable with those obtained using the original TEAC assay. Third, it is applicable to both aqueous and lipophilic systems.
Designs are generated which have an equally spaced distribution of points lying on concentric spherical shells. They have uniform space-filling properties and are tabulated up to ten factors. The designs are shown to be more uniform than familiar experimental designs on the basis of two measures of uniformity. Their use is illustrated by an example with four factors.
To evaluate the comparability of the two most common radical scavenging assays using 2,2′-azino-bis-3-ethylbenzthiazoline-6-sulphonic acid (ABTS) and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical, the 50 most popular antioxidant-rich fruits, vegetables and beverages in the US diet were identified and analyzed for their antioxidant capacities, total phenolics and flavonoids content. Spearmans–Rho correlation coefficients were calculated in order to characterize the relationship between antioxidant capacities, total phenolics and flavonoids content. Antioxidant capacity showed a strong positive relationship comparing both assays (ρ=0.949, p
Carob pulp kibbles, a by-product of carob been gum production, was studied as a source of bioactive agents. Firstly, the carob kibbles were submitted to an aqueous extraction to extract sugars, and supercritical fluid extraction (SFE) was applied to the solid residue of that aqueous extraction, by using compressed carbon dioxide (SC-CO2) as the solvent and a mixture of ethanol and water (80:20, v/v) as a co-solvent. Pressure and temperature were studied in the ranges 15–22MPa, and 40–70°C. Particle diameter, and co-solvent percentage in ranges of 0.27–1.07mm, and 0–12.4%, respectively, were also studied, as well as the flow rate of SC-CO2 between 0.28 and 0.85kgh−1, corresponding, respectively, to 0.0062 and 0.0210cms−1 of superficial velocity. The extracts were characterised in terms of antioxidant capacity by DPPH method, and total phenolics content by the Folin–Ciocalteu method. The central composite non-factorial design was used to optimise the extraction conditions, using the Statistica, version 6 software (Statsoft). The best results, in terms of yield and antioxidant capacity, were found at 22MPa, 40°C, 0.27mm particle size, about 12.4% of co-solvent and a flow rate of 0.29kgh−1 of SC-CO2. The phenolics profile of the extracts obtained at these conditions was qualitatively evaluated by HPLC-DAD. The solid residue of the supercritical extraction was also studied showing to be a dietary fiber, which can be compared to Caromax™, a carob fiber commercialised by Nutrinova Inc.
The growing interest in the substitution of synthetic food antioxidants by natural ones has fostered research on vegetable sources and the screening of raw materials for identifying new antioxidants. Oxidation reactions are not an exclusive concern for the food industry, and antioxidants are widely needed to prevent deterioration of other oxidisable goods, such as cosmetics, pharmaceuticals and plastics. Polyphenols are the major plant compounds with antioxidant activity, although they are not the only ones. In addition, other biological properties such as anticarcinogenicity, antimutagenicity, antiallergenicity and antiaging activity have been reported for natural and synthetic antioxidants. Special attention is focussed on their extraction from inexpensive or residual sources from agricultural industries. The aim of this review, after presenting general aspects about natural antioxidants, is to focus on the extraction of antioxidant compounds (mainly polyphenols) from agricultural and industrial wastes, as well as to summarize available data on the factors affecting their antioxidant activity and stability, and, in some cases, the reported major active compounds identified.
The benzoic and cinnamic acids found in forages were tested for their inhibitory effects on digestion of cellulose and hemicellulose by mixed cultures of rumen microorganisms in vitro. Rate and extent of cellulose digestion with the addition of cinnamic acids were determined. The benzoic acids and aldehydes were also compared for their inhibitory potential. Of the benzoic acid derivatives, only the parent compound (benzoic acid) inhibited in vitro dry matter disappearance (IVDMD) of cellulose after 48 h, whereas most of the cinnamic acids were inhibitory. None of these compounds depressed IVDMD of hemicellulose. Extent of cellulose digestion was unaffected by cinnamic acids, but rate of digestion was significantly reduced. The ranking of compounds for inhibitory potential was essentially reversed between 48 and 168 h of fermentation as compared with the ranking for 0 to 48 h of fermentation. There were also shifts in the molar proportions of volatile fatty acids produced between these times. The rapid reduction in concentration of cinnamic acids by microbial fermentation may explain these shifts. Benzoic aldehydes were more inhibitory of structural carbohydrate fermentation than were acids. No clear relationship existed between addition of hydroxyl or methoxyl groups to benzoic or cinnamic acids and their depressing effects on IVDMD. Cinnamic acids, which are more abundant in forages, were more inhibitory than the benzoic acids; but for all compounds, it appeared that hemicellulolytic bacteria were generally more tolerant of these compounds than the cellulolytic bacteria.
A method for the screening of antioxidant activity is reported as a decolorization assay applicable to both lipophilic and hydrophilic antioxidants, including flavonoids, hydroxycinnamates, carotenoids, and plasma antioxidants. The pre-formed radical monocation of 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS*+) is generated by oxidation of ABTS with potassium persulfate and is reduced in the presence of such hydrogen-donating antioxidants. The influences of both the concentration of antioxidant and duration of reaction on the inhibition of the radical cation absorption are taken into account when determining the antioxidant activity. This assay clearly improves the original TEAC assay (the ferryl myoglobin/ABTS assay) for the determination of antioxidant activity in a number of ways. First, the chemistry involves the direct generation of the ABTS radical monocation with no involvement of an intermediary radical. Second, it is a decolorization assay; thus the radical cation is pre-formed prior to addition of antioxidant test systems, rather than the generation of the radical taking place continually in the presence of the antioxidant. Hence the results obtained with the improved system may not always be directly comparable with those obtained using the original TEAC assay. Third, it is applicable to both aqueous and lipophilic systems.
We extracted polyphenols from carob (Ceratonia siliqua L.) pods, and evaluated the in vitro antioxidant activity of the crude polyphenol fraction (CPP). The total polyphenol content in CPP determined by the Folin-Ciocalteu method was 19.2%. The condensed tannin content determined by the vanillin and proanthocyanidin assay systems was 4.37% and 1.36%, respectively. beta-Carotene bleaching, 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging, inhibition of lipid peroxidation by the erythrocyte ghost, and microsomal assay systems were used to evaluate the antioxidant activity. CPP showed a stronger inhibitory effect against the discoloration of beta-carotene than other polyphenol compounds such as catechins and procyanidins. CPP had weaker antioxidant activity in the DPPH free radical scavenging, the erythrocyte ghost, and microsomal systems than authentic polyphenol compounds at the same concentrations. The activity adjusted by the polyphenol concentration was, however, comparable to that of authentic polyphenol compounds. Considering most carob pods are discarded and not effectively utilized at present, these results suggested that carob pods could be utilized as a functional food or food ingredient.
Extracts from pods and leaves of carob (Ceratonia siliqua L.) were tested for their ability to inhibit cell proliferation of mouse hepatocellular carcinoma cell line (T1). The two extracts showed a marked alteration of T1 cell proliferation in a dose-related fashion reaching the maximal effect at 1 mg/ml. Moreover, we demonstrated that leaf and pod extracts were able to induce apoptosis in T1 cell lines after 24-h treatment mediating a direct activation of the caspase 3 pathway. HPLC analysis revealed the presence of gallic acid, (-) epigallocatechin-3-gallate and (-) epicatechin-3-gallate in pod and leaf extracts, compounds well known to exert antiproliferative effects. Their concentration reached 6.28 mg/g in carob leaves and 1.36 mg/g in carob pods extract. The discovery that carob pod and leaf extracts contained antiproliferative agents could be of practical importance in the development of functional foods and/or chemopreventive drugs.
The polyphenolic patterns of carob pods (Ceratonia siliqua L.) and derived products were identified and quantified using high-performance liquid chromatography-UV absorption-electrospray ion trap mass spectrometry after pressurized liquid extraction and solid-phase extraction. In carob fiber, 41 individual phenolic compounds could be identified. In addition, spectrophotometric quantification using the Folin-Ciocalteu and vanillin assays was performed, and the antioxidative activity was determined as the 1,1-diphenyl-2-picrylhydrazyl radical scavenging activity. Carob pods contain 448 mg/kg extractable polyphenols comprising gallic acid, hydrolyzable and condensed tannins, flavonol-glycosides, and traces of isoflavonoids. Among the products investigated, carob fiber, a carob pod preparation rich in insoluble dietary fiber (total polyphenol content = 4142 mg/kg), shows the highest concentrations in flavonol-glycosides and hydrolyzable tannins, whereas roasted carob products contain the highest levels of gallic acid. The production process seems to have an important influence on the polyphenolic patterns and quantities in carob products.
Antioxidant activity of carotenoids is suggested to be one of the factors for their disease preventing effects. Marine carotenoids fucoxanthin and its two metabolites, fucoxanthinol and halocynthiaxanthin, have been shown to exhibit several biological effects. The antioxidant activities of these three carotenoids were assessed in vitro with respect to radical scavenging and singlet oxygen quenching abilities. The 1,1-diphenyl-2-picrylhydrazyl radical scavenging activity of fucoxanthin and fucoxanthinol was higher than that of halocynthiaxanthin, with the effective concentration for 50% scavenging (EC 50) being 164.60, 153.78, and 826.39 microM, respectively. 2,2'-Azinobis-3-ethylbenzo thizoline-6-sulphonate radical scavenging activity of fucoxanthinol (EC 50, 2.49 microM) was stronger than that of fucoxanthin (EC 50, 8.94 microM). Hydroxyl radical scavenging activity as measured by the chemiluminescence technique showed that the scavenging activity of fucoxanthin was 7.9 times higher than that by fucoxanthinol, 16.3 times higher than that by halocynthiaxanthin, and 13.5 times higher than that by alpha-tocopherol. A similar trend was observed when the hydroxyl radical scavenging was assessed by the electron spin resonance (ESR) technique. ESR analysis of the superoxide radical scavenging activity also showed the superiority of fucoxanthin over the other two carotenoids tested. Singlet oxygen quenching ability of the three carotenoids was lower than that of beta-carotene, with quenching rate constants ( k Q, x10 (10) M (-1) s (-1)) being 1.19, 1.81, 0.80, and 12.78 for fucoxanthin, fucoxanthinol, halocynthiaxanthin, and beta-carotene, respectively. The higher radical scavenging activity of fucoxanthin and fucoxanthinol compared with halocynthiaxanthin is assumed to be due to presence of the allenic bond.
Although it is already known that carob fibre contains several classes of polyphenolic substances, a comprehensive analysis of these has not been conducted to date. Therefore, the major polyphenolic compounds were extracted with organic solvents, and, following fractionation by normal-phase column chromatography on silicic acid, their structures were elucidated by liquid-chromatography electrospray-ionisation mass spectrometry (LC-ESI), nano-electrospray-ionisation mass spectrometry (ESI-MS), and gas-chromatography mass spectrometry (GC-MS). In addition, complete 1H and 13C NMR assignments were obtained for the isolated gallotannins 1,6-di-, 1,2,6-tri- and 1,2,3,6-tetra-O-galloyl-beta-D-glucose. Carob fibre was found to contain a rich variety of phenolic antioxidants. A total of 24 polyphenol compounds were identified with a yield of 3.94 g/kg (dry weight). The profile was dominated by gallic acid in various forms: free gallic acid (42% of polyphenols by weight), gallotannins (29%), and methyl gallate (1%), while simple phenols, mainly cinnamic acid, made up about 2% of the total. Flavonoids represented 26% of the polyphenols, and the major components were identified as the glycosides myricetin- and quercetin-3-O-alpha-L-rhamnoside (ca. 9% and 10%, respectively). These data indicate that carob fibre is rich in both amount and variety of phenolic antioxidant substances, and its inclusion in the diet may have chemopreventive properties.
Estudo da Produç ão de Manitol a partir de Xaropes de Alfarroba
- P Moniz
Moniz, P., 2008. Estudo da Produç ão de Manitol a partir de Xaropes de Alfarroba. MSc Thesis. Instituto Superior de Estudos Interculturais e Transdisciplinares-Instituto Piaget, Almada, Portugal.
Green tea catechins during food processing and storage: a review on stability and detection
- V K Ananingsih
- A Sharma
- W Zhou
- M G Bernardo-Gil
- R Roque
- L B Roseiro
- L C Duarte
- F Gírio
Ananingsih, V.K., Sharma, A., Zhou, W., 2011. Green tea catechins during food processing and storage: a review on stability and detection. Food Res. Int., http://dx.doi.org/10.1016/j.foodres.2011.03.004. Bernardo-Gil, M.G., Roque, R., Roseiro, L.B., Duarte, L.C., Gírio, F., Esteves, P., 2011. Supercritical extraction of carob kibbles (Ceratonia siliqua L.). J. Supercrit. Fluids 59, 36–42.
Flavonoids from Cynara cardunculus as possible markers. In: Characterisation and authentication of Serpa cheese
- L B Roseiro
Roseiro, L.B., 2003. Flavonoids from Cynara cardunculus as possible markers. In: Characterisation and authentication of Serpa cheese. Ph.D. Thesis. University of Reading, UK, pp. 145–151.