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Optimization of ultrasound-assisted extraction of anthocyanins in red raspberries and identification of anthocyanins in extract using high-performance liquid chromatography-mass spectrometry

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Abstract

Anthocyanins (Acys) are naturally occurring compounds that impart color to fruit, vegetables and plants. The extraction of Acys from red raspberry (Rubus idaeus L. var. Heritage) by ultrasound-assisted process (UAP) was studied. A central composite rotate design (CCRD) was used to obtain the optimal conditions of ultrasound-assisted extraction (UAE), and the effects of operating conditions, such as the ratio of solvents to materials, ultrasonic power and extraction time, on the extraction yield of Acys were studied through response surface methodology (RSM). The optimized conditions of UAE were as follows: ratio of solvents to materials was 4:1 (ml/g), extraction time was 200s, and ultrasonic power was 400 W. Under these conditions 34.5 mg of Acys from 100g of fresh fruits (T(Acy), expressed as cyanidin-3-glucoside), approximately 78.13% of the total red pigments, could be obtained by UAE. The Acys compositions of extracts were identified by high-performance liquid chromatography-mass spectrometry (HPLC-MS), 12 kinds of Acys had been detected and eight kinds of Acys were characterized. Result indicated that cyanidin-3-sophoroside, cyanidin-3-(2(G)-glucosylrutinoside), cyanidin-3-sambubioside, cyanidin-3-rutinoside, cyanidin-3-xylosylrutinoside, cyanidin-3-(2(G)-glucosylrutinoside), and cyanidin-3-rutinoside were main components in extracts. In addition, in comparison with the conventional solvent extraction, UAE is more efficient and rapid to extract Acys from red raspberry, due to the strong disruption of fruit tissue structure under ultrasonic acoustic cavitation, which had been observed with the scanning electron microscopy (SEM). However, the Acys compositions in extracts by both methods were similar, which were investigated using HPLC profile.

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... Comparing MAE and UAE, it was revealed that the second method exhibited higher yields regardless of the solvent used. It is known that the mechanical effects of ultrasounds result in the greater penetration of the solvent into the cellular matrix in a short time, thus improving the mass transfer and recovery of bioactive compounds [31,38,39]. ...
... The EYs of the untreated and dried samples extracted with CE using water and methanol are shown in Figure 3a, while the respective EYs of SE are shown in Figure 3b. result in the greater penetration of the solvent into the cellular matrix in a short time, thus improving the mass transfer and recovery of bioactive compounds [31,38,39]. ...
... However, both techniques presented significantly lower yields than MAE and UAE, with UAE being the best-performing technique. The mechanical effects of sonication seem to decrease the reliance on the solvent itself, improving the desorption of chemicals from the matrix and increasing the yield, especially when using methanol, in which more compounds are soluble [38]. ...
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In this study, solid olive mill waste (SOMW) was used to obtain antioxidant compounds using solid–liquid extraction. The effect of different extraction methods, namely microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), Soxhlet, and conventional solvent extraction, on the yield, total phenolics, and total antioxidant activity of SOMW extracts was investigated. Untreated and dried SOMW were subjected to extraction with water and methanol. The antioxidant activity of the extracts was evaluated using the DPPH assay, while their total phenolic content was measured using the Folin–Ciocalteu method. For the characterisation of the extracts, HPLC-DAD analysis was performed. The results showed that the extraction yield was significantly influenced (p < 0.05) by the solvent used, the material treatment prior to extraction, the moisture content of SOMW samples, and the extraction time. The optimised parameters were water, as the extraction solvent, and MAE as the extraction technique (extraction temperature of 50 °C and time of 1 h). The evaluation of the antioxidant activity of the extracts indicated that phenolics were the dominant bioactive compounds. The extracts were found to be rich in several hydroxytyrosol derivatives. Therefore, SOMW can be a valuable resource for bioactive compounds using conventional and innovative extraction techniques.
... When solid to liquid ratio increases it establishes a higher gradient of mass transfer between the solid and liquid which facilitates the diffusion of compounds. Additionally, it also increases the contact area between the matrix and the solvent and penetrates further in to extract higher quantity of anthocyanins [30]. A lower solid to liquid ratio could not yield higher TAC due to the fact that, lower volume of solvent is insufficient to fill up the flower matrix and the hypertonic environment could not be created, holding up the color in the vacuole of the material. ...
... We greatly acknowledge the financial assistance provided by National Research Council (19)(20)(21)(22)(23)(24)(25)(26)(27)(28)(29)(30)(31)(32)(33) ...
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Cassia fistula is a well-known plant species for the medicinal use of it leaves, barks and flowers. It has been identified as a rich source of phenolics which can be attributed to its medicinal properties. However, these phenolics should be extracted appropriately to effectively utilize them in various applications. This study focused on maximizing the extraction yield of total phenolics and total anthocyanins along with maximum 2,2-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity from edible flowers of C.fistula as a function of solid:liquid ratio, ethanol concentration, extraction temperature and time. The data was subjected to response surface methodology and the corresponding second order polynomial models were generated. The results showed that the polynomial models for all responses were significant, did not show lack of fit and presented determination of coefficients above 95%. This indicates the suitability of the models for prediction purposes. Using desirability function, the optimum extraction process parameters to obtain maximum values of all responses was found to be 29.56% ethanol, 1:45 solid to liquid ratio at extraction temperature of 31°C and time 24 minutes. Under these optimal conditions, the experimental values were in close agreement with the predicted values and did not show any significant difference (p<0.05). The identified optimized conditions could be used to extracts phenolics from C.fistula flowers in a cost effective and efficient manner.
... decoction (DCE) and maceration (MCE) (Vongsak et al., 2013) [57] and two modern methods viz. microwave assisted extraction (MAE) (Dahmoune et al., 2015) [18] and ultrasonic assisted extraction (UAE) (Chen et al., 2007) [14] . The procedure followed is as described by Yoganandi et al., (2018) [63] . ...
... decoction (DCE) and maceration (MCE) (Vongsak et al., 2013) [57] and two modern methods viz. microwave assisted extraction (MAE) (Dahmoune et al., 2015) [18] and ultrasonic assisted extraction (UAE) (Chen et al., 2007) [14] . The procedure followed is as described by Yoganandi et al., (2018) [63] . ...
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... Using temperatures higher than 60°C might lead to the degradation of phenolic compounds (Ju and Howard, 2003). Chen et al. (2007) reported that when the extraction temperature reaches above 60°C, a reduction in the phenolic content is observed, which is due to the destruction of some of the heat-sensitive compounds (Chen et al., 2007). Yingngam et al. (2015) studied the optimization of the process parameters of the extraction of phenolic compounds from the Cratoxylum formosum leaves using RSM. ...
... Using temperatures higher than 60°C might lead to the degradation of phenolic compounds (Ju and Howard, 2003). Chen et al. (2007) reported that when the extraction temperature reaches above 60°C, a reduction in the phenolic content is observed, which is due to the destruction of some of the heat-sensitive compounds (Chen et al., 2007). Yingngam et al. (2015) studied the optimization of the process parameters of the extraction of phenolic compounds from the Cratoxylum formosum leaves using RSM. ...
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Propolis is one of the byproducts of honey bees; it contains many phenolic compounds which are some of the most important natural antioxidants. The present study examined the antioxidant activity of propolis and its role in the stability of sunflower oil as a natural antioxidant in the form of Box-Behnken design. The extraction process was performed using an ultrasonic bath method with two factors in three levels which included 18 assays by the response surface methods. The investigated variables included the concentration of the extract (min: 30 and max: 1000ppm), the extraction time (min: 10 and max: 30 minutes), and temperature (min: 37.5 and max: 50°C). After analysis of the data in optimal conditions, the concentration of propolis ethanol extract, extraction temperature, and extraction time was determined as 997.5ppm, 34.6°C, and 30 min, respectively. In this condition, the total phenolic compounds and the free-radical scavenging properties were reported as 253.1mgGAE/100gDW and 85.9%, respectively. The result of the evaluation of the oxidative stability of the optimized sample oil showed reduced peroxide and thiobarbituric acid index compared to the control sample and synthetic antioxidants (BHT); also, the oil stability improved significantly over time.
... Table 3 shows the efficacy of the extraction process, in which the extracts treated with the HPST treatment showed high recovery of phenolic compounds content in a short treatment time (<2 min and 7 s), suggesting that the interaction of the high nominal power, short processing time and moderate-temperature had a positive effect in the extraction yield. These results agree with previously reported by Chen et al. [34], which showed that the short extraction time of 200 s associated with the high ultrasound power of 400 W resulted in the high recovery of anthocyanins from red raspberries. Therefore, our findings indicate that HIUS employing high-power and short-time treatments promotes the recovery of high phenolic contents reducing extraction time. ...
... The acoustic cavitation improves the direct migration of the target components into the surrounding solvent, increasing the mass transfer rate for bioactive compounds and the extraction yield. Chen et al. [34] optimized the HIUS-assisted extraction of anthocyanins from red raspberry. In the optimized condition (high power and short time; 400 W and 3.3 min), the tissue structure's scanning electron microscopy indicated the development of microfractures and disruption of cell wall due to the acoustic cavitation. ...
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This study aimed to evaluate the effects of the high-intensity ultrasound (HIUS) on the recovery of phenolic compounds from the leaves, fruit pulp, and seed of Eugenia calycina Cambess. The impact of using different modes of application of the same ultrasound-specific energy (kJ/g) was examined. Ultrasound energy performance was assessed employing two different HIUS treatments for each part plant. The same specific energy levels of 2 and 5 kJ/g were applied, varying nominal power and processing time. The HIUS treatments of low-power and long-time (LPLT) and high-power and short-time (HPST) were performed at 100 W, and 475 W. LPLT treatment was non-thermal processing, while HPST was a thermal treatment. The HPST treatment showed more efficiency in the recovery of the phenolic compounds to specific energies. The leaves were the plant part that exhibited the highest content of phenolic compounds and antioxidant activity. The LC-MS analysis also showed ellagic acid and myricitrin as the main phenolic compounds in all botanical parts evaluated. The SEM showed a physical change in plant structure because of HIUS. However, the FTIR spectra indicated that the chemical functional groups were not affected by the acoustic energy. Despite the HPST treatment increased the medium temperature, the stability of antioxidant compounds was preserved. The interaction of the high nominal power, short processing time, and moderate temperature employed in the HPST extraction procedure positively affected the extraction yield of phenolic compounds from the Eugenia calycina.
... The emergence of the above two situations might be related to two reasons. First, ultrasound waves with appropriate power agitated the extraction solvent and produced cavitation bubbles, which not only increased the pressure of the entire extraction system, but also promoted the contact between cellulase and raw materials, so that the combined action of the two made the cell wall more easily decomposed and broken [27,28]. Second, the excessive increase of power also promoted the generation of more chemical decomposition related to polysaccharides, resulting in the decline of extraction rate [29]. ...
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Response surface methodology was selected to explore the ultrasonic-assisted cellulase extraction conditions of Garcinia mangostana rind polysaccharides (GMRPs), and the optimum values of each condition were as follows: ratio of raw material to liquid of 1:50 g/mL, ultrasonic time of 40 min, enzyme concentration of 4 %, and ultrasonic power of 179 W. Based on the above conditions, the average extraction rate of GMRPs was 15.56 %. GMRPs were modified by carboxymethylation, and the relationship between the amount of chloroacetic acid and the substitution degree of carboxymethylated derivative was compared. Based on the results of single factor experiment, it was shown that the amount of chloroacetic acid significantly affected the degree of substitution of derivative products. The above research provides some valuable theoretical references for the preparation of GMRPs and its carboxymethylation products.
... In the study of Wang et al. [209], the increase of solvent used enhanced the flavonoid extract until the point 1:30 w/v, and then the yield decreased. Similarly, although several solid-to-solvent ratios from low to high were used to isolate bioactive compounds, the optimum conditions were not at the highest ratio but at a specific value, which was 1:4 w/v among from 1:1 to 1:7 w/v [210], or 1:8 w/v among 1:2 to 1:10 w/v [211]. ...
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The agriculture and horticulture industries generate many by-products while processing commodities, leading to significant environmental and societal dilemmas. Bioactive compounds obtained from by-products of plants are also known as ingredients in traditional medicines and the food industry due to their potential health benefits for humans as antioxidant, anti-inflammatory, and antimicrobial agents. On the other hand, an extensive array of colorants from natural sources has been scrutinized recently in different sectors to mitigate the negative ecological impacts of synthetic dyes, especially in modern textile manufacturing. Approaching these matters, this paper reviews various chemical compositions of plant secondary metabolites, including flavonoids, tannins, phenolic acids, essential oils, tulipalins, and factors that influence the isolation process. Moreover, the article offers an updated view of the advanced technologies for extraction, focusing on eco-friendly solvents such as water, supercritical carbon dioxide, and deep eutectic solvents. Eventually, a comparison of different extraction methods is highlighted to devise the most appropriate strategy for industries. Graphical abstract
... Raspberry pomace increases the red color levels of the wafers. This is due to the red pigment cyanide-3-sophoroside in them [1]. The main factor affecting the color changes of the wafers is the presence of anthocyanins in the raspberry pomace. ...
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Reducing waste products from the food industry has a positive impact on the environment and the economy. The appropriate amount of raspberry pomace in the production of wafers, has a significant impact on the physico-chemical, organoleptic and optical characteristics of these products. Literature data were used for supplementation of the research ingredient, ranging from 0 to 75 %. Informative characters that adequately describe the change in wafer characteristics upon addition of raspberry pomace were selected. Only 14 out of a total of 21 features were found to be sufficiently informative. Organoleptic characteristics, phenolic content and antioxidant activity, two color features from a laboratory model, color difference and yellow and brown indices can be considered as such. The three spectral indices included in the vector of informative features are sufficiently informative. A regression model was obtained describing the reduced experimental data with sufficient accuracy. An interior-point-legacy algorithm was used to determine the appropriate amount of raspberry pomace. The addition of 25,22 % raspberry pomace in wafers was found to have good organoleptic evaluation and nutritional value. The results obtained in this study can be used in the production of wafers with the addition of raspberry pomace, which will also enable the utilization of waste products from the production of this fruit in the food industry.
... The frequency of ultrasound in the extraction is efficient due to the breakdown of the cell wall; the implosion of cavitation bubbles generates microturbulence, high-speed collisions between particles, and internal diffusion (Perera and Alzahrani 2021;Shirsath et al. 2017). Furthermore, the power of ultrasound agitates the extraction solvent, thus increasing the contact between the solvent and the target compounds, significantly improving the extraction efficiency (Chen et al. 2007;Tena and Asuero 2022). ...
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Recently, growing demand for products enriched with natural compounds that support human health has been observed. Black rice, its by-products, and residues are known to have in their composition a large amount of these compounds with biological potential, mainly anthocyanins. These compounds have reported effects on anti-obesity, antidiabetic, antimicrobial, anticancer, neuroprotective, and cardiovascular disease. Therefore, the extract from black rice or its by-products have great potential for application as ingredients in functional foods, supplements, or pharmacological formulations. This overview summarizes the methods employed for the extraction of anthocyanins from both black rice and its by-products. In addition, trends in applications of these extracts are also evaluated regarding their biological potential. Commonly, the extraction methods used to recover anthocyanins are conventional (maceration) and some emerging technologies (Ultrasound-Assisted Extraction - UAE, and Microwave-Assisted Extraction - MAE). Anthocyanin-rich extracts from black rice have presented a biological potential for human health. In vitro and in vivo assays (in mice) showed these compounds mainly with anti-cancer properties. However, more clinical trials are still needed to prove these potential biological effects. Extracts from black rice and its by-products have great potential in applying functional products with beneficial characteristics to humans and reducing agro-industrial residues.
... 75 The major advantages of microwaves are higher extraction yields, shorter extraction times and higher selectivity. 76 Kashefi 77 compared the microwave extraction and hydrodistillation of Achillea millefolium EO, concluding that microwave extraction was more efficient than hydrodistillation. Also, Yang et al. 78 showed that microwave extraction was more effective than steam distillation in the case of Litsea cubeba EO, resulting in higher EO yield, possibly due to penetration of microwave waves into EO cells. ...
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... The extraction was done using two traditional methods viz., decoction (DCE) and maceration (MCE) (Vongsak et al., 2013) and two modern methods viz., microwave assisted extraction (MAE) (Dahmoune et al., 2015) and ultrasonic assisted extraction (UAE) (Chen et al., 2007). The procedure followed is as described earlier (Yoganandi et al., 2018, Donga andChanda, 2020). ...
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Abstract : The medicinal plants have been one of the major sources of medicines since the beginning of civilization. Herbal medicines are becoming more and more popular in recent years with their over increasing acceptability in both developing and developed countries. The development of new antimicrobial agents against resistant pathogens is increasing interest.In the present investigation, Ceiba pentandra (L.) Gaertn. seeds were extracted by Traditional and Modern extraction methods and evaluated their antibacterial and antifungal potential against some pathogenic microorganisms.The antibacterial and antifungal tests were performed using Agar well diffusion methodagainst 4Grampositive, 4 Gramnegative, 3 fungiand 3 clinical isolates. Antibacterial activity was more than antifungal activity. SA and EC were the most susceptible Gram positive and Gram negative bacteria while CR, CG and CN were the most resistant bacterial and fungal strains. The seed extracts may be a promising source of antimicrobics to treat microorganisms causing infectious diseases. They can be used as innovative antimicrobial agents thatare important in medicine and microbial control. Key Words : Ceiba pentandra, Seed, Extraction methods, Antibacterial, Antifungal, Agar well diffusion
... The majority of published studies emphasize the advantages of MAE and UAE for anthocyanins isolation in terms of enhancing the extraction efficiency while providing the shorter extraction time. For instance, UAE was shown to be more effective than conventional techniques for extraction of anthocyanins in red raspberry, blueberry wine pomace, and Hibiscus sabdariffa calyces [25][26][27]. Similarly, MAE showed to be more time and yield efficient in the isolation of anthocyanins from sour cherry, Chinese bayberry, blackberry, and black currant marc [22,[28][29][30]. ...
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Black chokeberry juice production results in a large amount of pomace, which is usually regarded as waste. Nevertheless, it contains significant amounts of anthocyanins, which can be utilized as health-promoting components, but also as food colorants. To take advantage of their benefits, green extraction methods such as microwave-assisted (MAE) and ultrasound-assisted extraction (UAE) are widely used for their isolation. This study aimed to evaluate the effects of MAE and UAE parameters (solvent, treatment time, temperature, or ultrasound amplitude) on the extraction yield of anthocyanins from black chokeberry pomace and to compare the effectiveness of these two green extraction methods with conventional reflux extraction, both in terms of total anthocyanins yield and effects on individual compounds. In both techniques, acidification of the extraction solvent did not show a significant effect on anthocyanin content. For MAE, a temperature increase from 40 to 60 °C positively affected the extraction yield, while 4 min was a substantial treatment time for the extraction. Conversely, UAE required 10 min of treatment time with no effect on amplitude. UPLC ESI-MS2 analysis confirmed the presence of 6 anthocyanins in the obtained extracts, with significantly higher levels of cyanidin-3-O-xyloside and cyanidin-3-O-arabinoside were in ones isolated by green extraction techniques.
... They showed that similar amounts of phenolic compounds could be extracted from strawberries in 2 min, whereas it took 20 h with a conventional method and 3 h using supercritical fluid extraction. Another example is the extraction of anthocyanins from raspberries, a process developed by Chen et al. (2007). In this study, the same yields of anthocyanins were reached in 3 min when using UAE compared with 53 min with a conventional extraction system. ...
... In the literature, there are some works involving the extraction of bioactive compounds from raspberries, as well as studies on extraction optimization using different technologies (Suthanthangjai et al. 2005;F. Chen et al. 2007;Sun et al. 2007;Mihailović et al. 2019;Wang et al. 2019). However, it is important to emphasize that the content of bioactive compounds present in raspberries can be influenced by several factors, mainly genetic and environmental (Bowen-Forbes et al. 2010;Çekiç and Özgen 2010;Bobinait et al. 2012;Yang et al. 2020). Furthermore, comprehen ...
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Bioactive compounds are of considerable interest due to their antioxidant properties and potential beneficial health effects. Thus, this study aimed to optimize and model the ultrasound-assisted extraction process (UAE) of response variables total anthocyanins (TA) and total phenolic content (TPC) from raspberries, and to compare the optimized extraction process with the conventional one. The variables used were time (5 to 75 min), temperature (30 to 70 °C), and solid: liquid ratio (1:5 to 1:15 m/v), applied to the Box-Behnken Design. The optimal condition of the UAE process occurs at a temperature of 70 °C and a solid: liquid ratio of 1:12.5 m/v, for both response variables. The optimal time for extraction of TA occurs in 22.5 min predicting the content of 23.181 mg/100 g and for TPC occurs in 57.5 min predicting the content of 156.30 mg GAE/100 g. On validation of the optimized conditions, less than a 5% difference was found between the predicted and experimental values (24.131 mg/100 g for TA, and 149.226 mg GAE/100 g for TPC). When comparing the optimized UAE with the conventional extraction, it wares observed that UAE increased (p < 0.05) the extraction of TA content by 18.28% and TPC by 28.88%. The process time reduction from 24 h in conventional extraction to less than 1 h in optimized UAE stands out. Furthermore, the Film Theory model tested fitted well to the extraction process under study. Thus, the study indicates that the UAE process is an efficient green methodology for recovering bioactive compounds from raspberries.
... This technique can overcome some of the disadvantages of conventional HD. For example, the treatment can overcome the challenges of long extraction times and low-efficiency problems (Chen et al., 2007). HD can increase EO yields, as demonstrated in the following research works: Liu et al., 2019 (Iberis Amara seeds); Chen, Sun, et al., 2020 (Cinnamomum cassia bark); Boubechiche et al., 2017 (Allium sativum); Zorga et al., 2020 (Celery Seeds); and Chen, Liu, et al., 2020 (leaves of Perilla frutescens). ...
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Spearmint essential oil (SEO), one of the economically valuable natural products, has special importance in the food, pharmaceutical, and perfumery industries due to its antifungal, antioxidant, and enzyme inhibitory properties. In this study, we optimized and evaluated the effect of three pre‐treatments on the extraction of SEO for quantity and quality: ultrasonic bath (UB), water to material ratio‐ultrasonic bath (W/M‐UB), and cold plasma‐ultrasonic bath (CP‐UB). Three experiments were designed using the central composite design (CCD) of response surface methodology (RSM). Experimental treatments included UB temperature (30–80°C) and time duration (1–30 min), cold plasma (CP) power (15–24 kV), and water/material ratio (10–40). Then, SEOs were extracted by hydro‐distillation using the Clevenger apparatus. The results showed that SEO yield in the optimal conditions of treatments was 119.7%, 206.6%, and 155.7% higher in UB, W/M‐UB, and CP‐UB pretreatments respectively, in comparison to control sample and optimized conditions were UB temperature: 37.3°C and UB time: 5.2 min at UB treatment, 33.9 of W/M ratio, 69.9°C of UB temperature and 6.9 min of UB time at W/M‐UB treatment and CP power: 22.176, UB temperature: 40.135 and UB time: 24.122 at CP‐UB treatment. Oxygenated monoterpenes were also higher in the essential oils (EOs) of all three treated plant materials. In conclusion, the SEO extraction yield improved by the application of the pretreatments in optimized conditions. The aim of this study was to increase the extraction efficiency of essential oil. Treatments were ultrasonic bath, water to material ratio, and cold plasma. Increasing the time of ultrasonic bath and cold plasma power led to a higher yield. Treatments with ultrasonic bath temperature and water/material ratio inversely affected the yield. The treatments raised the percentage of oxygenated monoterpenes slightly.
... Pelargonidin acylated derivatives and glycosides were reported in the literature from red raspberries. The quantity of anthocyanins varies from 0.1 to 134 mg/100 g FW, 76 to 365 mg/100 g DW, and 336 to 1030 mg/100 g DEW [15,89,97,102,117,132,152,153,[158][159][160][161]169,170] of red raspberry variety. Reported studies indicate usage of acidified (HCl or formic acid) methanol alone or ethyl acetate extraction followed by acidified methanolic extraction for the qualitative/quantitative analysis of anthocyanins is suitable for the red variety. ...
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Anthocyanins are reported to exhibit a wide variety of remedial qualities against many human disorders, including antioxidative stress, anti-inflammatory activity, amelioration of cardiovascular diseases, improvement of cognitive decline, and are touted to protect against neurodegenerative disorders. Anthocyanins are water soluble naturally occurring polyphenols containing sugar moiety and are found abundantly in colored fruits/berries. Various chromatographic (HPLC/HPTLC) and spectroscopic (IR, NMR) techniques as standalone or in hyphenated forms such as LC-MS/LC-NMR are routinely used to gauge the chemical composition and ensure the overall quality of anthocyanins in berries, fruits, and finished products. The major emphasis of the current review is to compile and disseminate various analytical methodologies on characterization, quantification, and chemical profiling of the whole array of anthocyanins in berries, and fruits within the last two decades. In addition, the factors affecting the stability of anthocyanins, including pH, light exposure, solvents, metal ions, and the presence of other substances, such as enzymes and proteins, were addressed. Several sources of anthocyanins, including berries and fruit with their botanical identity and respective yields of anthocyanins, were covered. In addition to chemical characterization, economically motivated adulteration of anthocyanin-rich fruits and berries due to increasing consumer demand will also be the subject of discussion. Finally, the health benefits and the medicinal utilities of anthocyanins were briefly discussed. A literature search was performed using electronic databases from PubMed, Science Direct, SciFinder, and Google Scholar, and the search was conducted covering the period from January 2000 to November 2022.
... The anthocyanin components of skin were extracted according to the method of Chen et al. (2007) with slight modification. Under dark conditions, 0.5 g of frozen red and green skin samples were ground on ice, dissolved in 1.5 mL of 1% HCl-methanol, mixed until homogenized, and extracted at 4°C for 12 h. ...
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Biostimulants play an important role in promoting crop growth and development and improving fruit yield, but their influence on fruit quality in horticulture plants is still unclear. In this study, four types of biostimulants, Ainuo (AN), Aigefu (AG), Weiguo (WG), and Guanwu Shuang (GS) were applied to the fruit surface of ‘Yinhongli’ plum at 60 and 75 days after anthesis to investigate their effect on carbohydrates and biosynthesis of anthocyanins, and also analyze the relationship between sugar and anthocyanin accumulation during fruit color change to ripening. Results showed that all biostimulant treatments significantly improved fruit appearance quality, and increased single fruit weight and TSS/TA. Cyanidin 3- O -glucoside and cyanidin 3- O -rutinoside, are the most important anthocyanins in the red skin of the ‘Yinhongli’ plum, and no anthocyanin was detected in the green skin. In addition, WG and GS treatments significantly increased the expression of structural genes involved in anthocyanin biosynthesis compared with the control, especially chalcone synthase (CHS) and flavonoid 3-O-glucosyltransferase (UFGT) at 95-105 d after anthesis, leading to anthocyanin accumulation 10 days earlier than the control. Correlation analysis showed that there was a significant correlation between total sugar and anthocyanin content during fruit coloring and ripening.
... Based on the observation for the yield of anthocyanins, TAC has increased from 0.53 to 1.58 mg cy-3-glu /g DW when varying the temperature from 20 °C to 45 °C, further increase in temperature decreased the yield up to 0.32 mg cy-3-glu/g DW. Results from the previous works on blueberry wine pomace, red raspberry and black currants (He et al., 2016;Chen et al., 2007;Cacace and Mazza, 2003) have revealed similar outcomes, where yield of anthocyanins increased up to certain temperature and significantly reduced upon further increase in temperature. Though moderate temperature ranges increase mass transfer rates of anthocyanins by increasing compound solubility and diffusivity, anthocyanins are relatively unstable at high temperatures. ...
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More and more people are becoming curious about the benefits of using natural dyes in textiles. Toxic and allergic reactions associated with synthetic dyes have prompted many countries to establish stringent environmental regulations. Natural dyes are more biodegradable and environmentally friendly than synthetic dyes. There are four types of natural dyes: those originating from plants, animals, minerals, and microorganisms. All natural fabrics can be dyed using natural dyes. They can also be used to color synthetic fabrics, according to a recent study. Natural dyes aren't just for textiles; they're used in food, medicine, handicrafts, and leather processing. Many of the plants that provide natural color are also used in traditional medicine. The classification of natural dyes and the numerous sustainability challenges associated with their manufacture and application are reviewed in this paper in an attempt to be comprehensive.
... mg C3G per 100 g of fw), black currants (62.80-271.33 mg C3G per 100 g of fw), red grapes (0.30-164.20 mg C3G per 100 g of fw), and red raspberries (21.90-62.50 mg C3G per 100 g of fw) [64][65][66][67][68][69][70]. In addition, sour and sweet cherries also have significant amounts of anthocyanins, with TAC values ranging from 10.50-87.40 ...
Article
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Anthocyanins are among the best-known phenolic compounds and possess remarkable biological activities, including antioxidant, anti-inflammatory, anticancer, and antidiabetic effects. Despite their therapeutic benefits, they are not widely used as health-promoting agents due to their instability, low absorption, and, thus, low bioavailability and rapid metabolism in the human body. Recent research suggests that the application of nanotechnology could increase their solubility and/or bioavailability, and thus their biological potential. Therefore, in this review, we have provided, for the first time, a comprehensive overview of in vitro and in vivo studies on nanocarriers used as delivery systems of anthocyanins, and their aglycones, i.e., anthocyanidins alone or combined with conventional drugs in the treatment or management of chronic diseases.
... mg C3G per 100 g of fw), black currants (62.80-271.33 mg C3G per 100 g of fw), red grapes (0.30-164.20 mg C3G per 100 g of fw), and red raspberries (21.90-62.50 mg C3G per 100 g of fw) [64][65][66][67][68][69][70]. In addition, sour and sweet cherries also have significant amounts of anthocyanins, with TAC values ranging from 10.50-87.40 ...
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Anthocyanins are among the best-known phenolic compounds and possess remarkable biological activities, including antioxidant, anti-inflammatory, anticancer, and antidiabetic effects. Despite their therapeutic benefits, they are not widely used as health-promoting agents due to their insta-bility, low absorption, and thus, low bioavailability and rapid metabolism in the human body. Recent research suggests that the application of nanotechnology could increase their solubility and/or bioavailability, and thus, their biological potential. Therefore, in this review, we decided to provide, for the first time, a comprehensive overview of in vitro and in vivo studies on nanocarriers used as delivery systems of anthocyanins, and their aglycones, i.e., anthocyanidins alone or com-bined with conventional drugs to the treatment or management of chronic diseases.
... Further interaction of time and temperature significantly affected the ABTS value (Table S4(d)). A lower range of temperature with a lower extraction time was more effective in the extraction of antioxidants from carrot rejects 48 . Hence the extraction conditions of microwave temperature of 40 °C, time of 5 min, and solid to solvent ratio (1:40) were the optimized results for the maximum ABTS value. ...
Article
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Carrot processing industries produce 25–30% of waste in the form of carrot rejects, peels, and pomace which contain a large amount of high-value bioactive components. Green extraction of the bioactive components from carrot rejects with green solvents using closed-vessel energy-intensive microwave-assisted extraction was the objective of this work. In this work, three experimental studies were implemented. One uses 8 different green solvents for maximum yield of bioactive using green technology, and the other for the optimization of Microwave-assisted Extraction (MAE) parameters to enhance the bioactive components yield. Response Surface Methodology was employed to optimize the processing parameters including temperature, time, solid to solvent ratio, and solvent type. The optimized extraction conditions: treatment temperature of 50 °C for 5 min gave a significantly higher yield of total carotenoids (192.81 ± 0.32 mg carotenoids/100 g DW), total phenolic (78.12 ± 0.35 g GAE/100 g DW), and antioxidants by FRAP (5889.63 ± 0.47 mM TE/100 g DW), ABTS (1143.65 ± 0.81 mM TE/100 g DW), and DPPH (823.14 ± 0.54 mM TE/100 g DW) using a solvent combination of hexane and ethanol (1:3) with solid to solvent ratio of 1:40 (w/v). This green technology in combination with GRAS solvents promoted the best recovery of bioactive from carrot rejects. Moreover, the solid residue remained after the extraction of bioactive components exhibited higher carbon content (46.5%) and calorific value (16.32 MJ/kg), showcasing its potential to be used as an energy source.
... UAE is based on the utilization of ultrasonic energy (sound waves with frequencies more than 20 kHz) to facilitate the extraction of analytes from a solid sample by the solvent [19,20]. The use of UAE offers advantages over the conventional method such as selectivity, low energy consumption, reduction in solvent consumption, and extraction time, and reduction in consumption of hazardous chemicals, among others [15,[21][22][23]. UAE has been used to extract phenolic compounds from different matrices, including Achillea arabica [24], spruce wood bark [25], Jatropha dioica, Eucalyptus camaldulensis [26], black chokeberry [27], and others [28][29][30][31]. ...
Article
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Welsh onion (Allium fistulosum) leaves contain several bioactive compounds that can be extracted and used to develop new value-added products (e.g., functional foods and dietary supplements). In the current work, optimal ultrasound-assisted extraction (UAE) conditions to obtain extracts with high polyphenols content and DPPH (1,1-diphenyl-2-picrylhydrazil) scavenging activity were identified using response surface methodology. A complete 3k factorial design was used to evaluate the effect of different variables of the UAE (extraction temperature, time, and ethanol concentration) on the polyphenols content and the DPPH scavenging activity of the extracts. The best conditions for UAE to reach both the highest values of total polyphenols content (51.78 mg GAE/100 g) and DPPH scavenging activity (34.07 mg Trolox equivalents/100 g) were an extraction temperature of 60 °C, time of 10 min, and ethanol concentration of 70% v/v. The antioxidant activity of the extracts obtained at the optimal conditions was also evaluated by 2,2′-azino-bis-3-ethylbenzthiazoline-6-sulphonic acid (ABTS) and ferric reducing antioxidant power (FRAP) assays obtaining values of 155.51 ± 2.80 μM Trolox/100 g and 1300.21 ± 65.55 μM Trolox/100 g, respectively. Moreover, these extracts were characterized by UHPLC-ESI+-Orbitrap-MS analysis finding that cyanidin (6.0 mg/kg) was the phenolic compound found in the highest amount followed by quercetin-3-glucoside (4.4 mg/kg).
... Values are mean ± standard deviation; the different letters above the bars indicate a significant difference at p < 0.05 for the ANOVA and Tukey post-hoc test mean comparisons. of ultrasound. Chen et al. [38] indicated a loosening of the berries' structure and an increase in the number of ruptured cells during ultrasonic treatment. This was due to acoustic cavitation and microjets, which can damage cellular material. ...
Article
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Combined vacuum impregnation and ultrasound was proposed as an alternative method to improve the infusion of ascorbic acid in berry fruit. The effect of ultrasound application at different stages of impregnation – vacuum, relaxation, and both stages – on the qualitative characteristics of impregnated cranberries was investigated. The quality assessment was based on porosity, color, antioxidant capacity, anthocyanin, polyphenol and structure compound content. Ultrasound-assisted vacuum impregnation contributed to higher ascorbic acid content, smaller relative color difference, and greater antioxidant properties. It was found that the degree of impregnation varies considerably and depends on the stage of using ultrasound. Due to more favorable quality attributes, the conclusion was reached that ultrasound should be applied during the relaxation stage of vacuum impregnation.
... Herrera et al. (2004) compared the efficiency of different extraction techniques on phenolic compounds of strawberry and showed that the UAE procedure took the least time compared to conventional and supercritical fluid extraction. Chen et al. (2007) studied the extraction of anthocyanins from raspberries by ultrasound using methanol as solvent and retrieved 78.13% of anthocyanins. A fast UAE method was developed by Barbero et al. (2008) for the extraction of capsaicinoids from the pepper. ...
Chapter
Ultrasound is an environment-friendly technology used in food processing, preservation, and extraction. Depending on the intensity of the ultrasound, the applications of ultrasound in the food industry can be either low-intensity or high-intensity ultrasound. Application in food ranges from degassing/defoaming of beverages to depolymerisation, demoulding, and extrusion/cooking. The ultrasonic transducer rotates at different speeds producing complex movement covering a large defoaming area. When the ultrasonic waves are applied to meat for cooking, it causes lesser loss of water and better attribute of the cooked meat. In the crystallization application, when the frequency of ultrasound is within the frequency of the relaxation of ice crystals in the food, the acoustic energy could be absorbed by frozen foods. In ultrasound- assisted drying application, a series of rapid and successive compressions and rarefactions are introduced in the food material that would accelerate the diffusion at the boundary between a suspended solid and a liquid. Thus the undesirable changes in the organoleptic properties of the food caused by thermal drying or dehydration are reduced. Ultrasound when applied to depolymerisation causes mechanical degradation of the polymer from collapsed cavitation bubble and chemical degradation as a result of the chemical reaction between the polymer and high energy molecules, such as hydroxyl radicals produced from the cavitation phenomenon. In the extrusion process, the use of ultrasound energy is a better alternative than the mechanical process to remove the adhered cooked food from the processing vessel surface. Tenderization of meat by ultrasound is done by the disruption of the cell membrane by weakening the muscle structure and activating proteolytic enzymes. Similarly, ultrasound is also effective in homogenization, sterilization, and all other processes of food preservation.
... A few extraction technologies, such as pressurized liquid extraction, have been developed to enable the rapid extraction of anthocyanins and other phenolics at high temperatures (>50 • C) [35], and they were found to be successful in retarding anthocyanin degradation during processing. It was also found that ultrasound-assisted solvent extraction was more efficient for extracting anthocyanin than conventional solvent extraction due to the strong disruption of the fruit tissue under ultrasonic acoustic cavitation [36]. ...
Article
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Anthocyanins are flavonoids with an antioxidant effect. They are the pigments that give rich colours to berries, red onions, pomegranates, and grapes. In addition to acting as antioxidants and fighting free radicals, anthocyanins may offer anti-inflammatory, anti-viral, and anti-cancer benefits. Among various types of fruits, blackberries and grapes are distinguished by their rich content in polyphenols, including anthocyanins. The purpose of this study was the identification and quantification of the anthocyanins in black grape skins and blackberries, but also the determination of the total phenolic content and total antioxidant capacity. The grape skins and blackberry extracts were prepared by an ultrasound-assisted acidified ethanol and methanol extraction method, with the 80% methanol solution being the most effective. Alcoholic extracts of blackberries and grape skins were analysed by the HPLC-DAD-MS method. There were five glycosylated anthocyanin compounds in blackberries, eight glycosylated anthocyanins compounds, and seven fragments of anthocyanin derivatives in grape skins identified. It was concluded that the anthocyanin profile of blackberries and grapes revealed mainly anthocyanin monoglycosides and acetylglycosides. Cyanidin-3-glucoside was the main component (86.49%) in blackberries, while, in the grape skins, the main component was delphinidin-3-O-glucoside (about 40.64%). Principal component analysis (PCA) was carried out on the basis of the 13 identified compounds in order to separate the extracts and describe the anthocyanins characteristics of different groups, the findings being in agreement with the experimental results. Compared to methanol extracts, ethanol extracts showed higher antioxidant activity, being related to the total phenolic content for the blackberries. Overall, the obtained results indicated that the blackberries and grapes skins possessed a high antioxidant content, similar to other berries, highlighting their potential use as fresh functional foods or fruit-derived products.
... C3S with 79% area under the peak (AUP), cyanidin-3-glucoside (15% AUP), and cyanidin-3-sambubioside (4% AUP) were the major ACNs identified from the PDA/MS-MS data and in comparison with those reported in the literature at 520 nm. 27,28 Small traces of ACN derivatives ( pelargonidin, peonidin and malvidin) were accounted for the remaining percentage area under the peak of the pigments, but could not be clearly identified due to the presence of co-eluting compounds (Table 1). These peaks were assigned aglycone identities based on selected ion monitoring. ...
Article
Berry fruits are rich in polyphenolic compounds (PCs) and may promote health benefits. Anthocyanin (ACN) concentrations of red raspberry (RR) (Rubus idaeus) extracts were 887.6 ± 262.8 μg g-1, consisting mainly of cyanidin-3-sophoroside (C3S) equivalents. To test the efficacy of RR in diabetes treatment, seven patients with type 2 diabetes mellitus (T2DM) were given one oral RR serving (123 g per day) for two weeks. Blood samples were drawn at the baseline (BSL) and post-feeding (PF) periods for phenolic metabolite, inflammation and insulin resistance (IR) biomarker analysis. Two urolithin conjugates, urolithin A glucuronide (Uro-A glur) and urolithin A sulphate (Uro-A sulf) were identified in the PF period in 5 of the 7 patients in nanomolar concentrations (1.6 ± 0.7-63.2 ± 31.2 nM). ACN-derived metabolites such as protocatechuic acid (PCA) and 3,4-dihydroxyphenylacetic acid (DOPAC) were at micromolar levels and were higher during the PF period for diabetics and the levels were as follows: BSL: PCA = 0.6 ± 0.4, DOPAC = 1.2 ± 0.5; PF: PCA = 0.6 ± 0.4, DOPAC = 1.1 ± 0.6. The results revealed significant reductions in high sensitivity C-reactive protein, hsCRP (p = 0.01) and there was a downward trend in IR measured by the homeostatic model assessment of insulin resistance (HOMA-IR, p = 0.0584) in T2DM patients. DOPAC (1-100 μM) failed to stimulate insulin secretion in pancreatic β-cells. The multiplex assay showed variations in the cytokine levels between patients, but differences were not significant. This study demonstrates a potential use of RR in the treatment of inflammation and possibly IR as well in patients with type 2 diabetes.
... In most cases, solvents are acidified with HCl or organic acids (formic acid, acetic acid, or trifluoroacetic acid) in different concentrations (Hohnova et al., 2017). Previous studies have used different extraction methods to obtain anthocyanin from various fruits and reported more efficient results in obtaining anthocyanin by employing the ultrasonic method (Chen et al., 2007;Ekici, 2011;Veggi et al., 2011). Anthocyanins, which have nutraceutical properties with the capability to inhibit free radicals, are used in food, cosmetics, and pharmaceutical products (Sengul et al., 2014). ...
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In this study, extracts were prepared from the flesh and seeds of Rosa pimpinellifolia L. using different solvents and different extraction methods. Flesh pulp, seed powder, and the obtained extracts were added to the ice cream at 5%. Changes in some physical and chemical properties of the ice cream at the beginning and in the 2nd, 4th, and 6th months of storage were determined. It was found that the process had a very significant effect on dry matter content, pH value, titratable acidity, volume increase, complete melting time, L*, a*, b*, C, Hº, and ΔE values, total phenolic content, and total monomeric anthocyanin content (p<0.01). It was revealed that storage time had a very significant effect on dry matter content, pH value, titratable acidity, complete melting time, b* and C values, total phenolic content, and ABTS•+ (p<0.01). There was no change in the total content of monomeric anthocyanins during the storage period of ice cream samples.
... This aids in production of cavitation bubbles by ultrasonic waves. Cavitation bubbles grows during refraction and rarefaction cycle of ultrasonic waves until it reaches a critical size, after which it Page | 63 erupts with a release of enormous amount of energy [233]. Released energy either enlarge the pores in call or disrupt the cell wall completely. ...
Thesis
Roots and Tuber crops plays an eminent, countless and complex part in feeding the world. These crops have the potential to eradicate poverty and improve food security. Starch is the principal component of roots and tuber crops. The significance of starch as a raw material in both food and non-food industries are increasing. In present study efficiency of ultrasound assisted extraction (UAE) to increase the yield of starch and polyphenols from lontan (Canna and Cassava) crops were analysed along with its influence on the physiochemical properties of extracted compounds. Extraction parameters (Temperature, time, solid: liquid ratio) were optimized through Box Behnken response surface design (BBD). Physiochemical and functional properties of starch and polyphenols were investigated through SEM, swelling and solubility index, oil and water absorption index, Total polyphenol yield, DPPH and ORAC assay. Starch yield obtained from canna and cassava at the optimum extraction conditions (Canna: temperature 40°C, time 10 min, solid: liquid ratio 1:30 g/ml; Cassava: temperature 40°C, time 10 min, solid: liquid ratio 1:25 g/ml) were 19.81% and 16.51% respectively. Obtained starch yield was found to be significantly higher than the yield attained through conventional extraction method without any significant or adverse changes in the physicochemical and functional properties. Total polyphenol yield from canna and cassava rhizome was 1061.72 mg GAE/&100g and 7644.46 mg GAE/&100g respectively. Total polyphenol yield obtained through UAE was found to be significantly higher than conventional method. Antioxidant activity of bioactive compounds analysed through DPPH and ORAC was found to be directly proportional to the attained polyphenol yield. From the obtained results it can be observed that UAE has the efficiency to increase the yield of starch and polyphenols without altering the properties of isolated compounds.
... The ultrasound-assisted technique is often used in polyphenols extraction [50][51][52] and consists of the shaking of the sample in the extraction solvent for extended periods of time [53]. During the treatment with ultrasounds, the cell wall matrix is disrupted and various compounds, including polyphenols, are released into the medium. ...
Article
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Cranberry is a fruit originally from New England and currently growing throughout the east and northeast parts of the USA and Canada. The supplementation of cranberry extracts as nutraceuticals showed to contribute to the prevention of urinary tract infections, and most likely it may help to prevent cardiovascular and gastroenteric diseases, as highlighted by several clinical trials. However, aiming to validate the efficacy and safety of clinical applications as long-term randomized clinical trials (RCTs), further investigations of the mechanisms of action are required. In addition, a real challenge for next years is the standardization of cranberry’s polyphenolic fractions. In this context, the optimization of the extraction process and downstream processing represent a key point for a reliable active principle for the formulation of a food supplement. For this reason, new non-conventional extraction methods have been developed to improve the quality of the extracts and reduce the overall costs. The aim of this survey is to describe both technologies and processes for highly active cranberry extracts as well as the effects observed in clinical studies and the respective tolerability notes.
... Therefore, optimization of ultrasound power is an important step. Chen et al. (2007) reported that the change of ultrasonic power and extraction time had a significant effect on the TAC of red raspberries extracts. In our study, at a low level of extraction time (13.86) and temperature (57.41 °C), maximum desirability was obtained. ...
Article
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Abstract This study aimed to investigate the potential use of anthocyanin of Berberis crataegina DC. as a natural food coloring agent in the food industry. For this aim, the ultrasound-assisted extraction (UAE) method was performed to extract anthocyanin of Berberis crataegina DC. The effect of ultrasound power (X1: 20-100%), extraction temperature (X2: 20-60 °C), and time (X3: 10-20 min) on TPC and TAC of Berberis crataegina DC. extracts were examined and optimized by applying the Box–Behnken experimental design (BBD) with the response surface methodology (RSM). The influence of three independent variables and their combinatorial interactions on TPC and TAC were investigated by the quadratic models (R2: 0.9638&0.9892 and adj R2:0.9171&0.9654, respectively). The optimum conditions were determined as the amplitude level of 98%, the temperature of 57.41 °C, and extraction time of 13.86 min. The main anthocyanin compounds were identified, namely, Delphinidin-3-O-galactoside, Cyanidin-3-O-glucoside, Cyanidin-3-O-rutinoside, Petunidin-3-O-glucoside, Pelargonidin-3-O-glucoside, and Peonidin-3-O-glucoside. The anthocyanin degradation showed first-order kinetic, degradation rate constant (k), the half-life values (t1/2), and loss (%) were significantly affected by different temperatures (P < 0.05). Higher degradation (k) in anthocyanin content was observed at 90 °C. This study suggested that UAE is an efficient method for the extraction of TPC and TAC from Berberis crataegina DC.
... is could be explained that when the pH and the extraction temperature were not too high, the impact of enzyme and high ultrasonic power efficiently broke the structure of the cell wall, leading to the diffusion of content of polysaccharides into solvent. However, at high pH (>8.2) and high temperature (>52 o C), the yield of polysaccharides experienced a decrease because polysaccharides were reported to be more likely to be hydrolyzed under these conditions [22,23]. is result is suitable with a previous study [24]. Figure 3 illustrates the simultaneous effects of pH and extraction time on content of polysaccharides while the ultrasonic power was of 360 W and extraction temperature was of 50°C. ...
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Red Ganoderma lucidum (G. lucidum) is a popular medicinal herb commonly used in Vietnamese traditional remedies due to its potential value for health. In this study, polysaccharides were extracted from G. lucidum using ultrasound-assisted enzymatic extraction method. The response surface methodology and Box–Behnken design were employed to investigate the effects of pH, extraction temperature, extraction time, and ultrasonic power on the content of polysaccharides. Based on ultraviolet-visible spectroscopy analysis, the highest content of polysaccharides in the extract was 32.08 mg/g under optimum experimental parameters including enzyme concentration of 3%, pH of 5.5, extraction temperature of 45°C, extraction time of 30 min, and ultrasonic power of 480 W. The Fourier-transform infrared spectroscopy was also used to identify the functional groups in the extracts. The molecular weights of polysaccharides were determined by gel permeation chromatography. The obtained extract was then evaluated for anticancer activities by using (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay, showing the anticancer activities with the half-maximal inhibitory concentration value of more than 512 μg/mL. This result suggested that UAEE could be considered as an appropriate and effective extraction method for bioactive crude polysaccharides from G. lucidum.
Article
Sorghum 3‐deoxyanthocyanins (3‐DXAs) have greater stability when compared to other anthocyanins. However, the efficiency in extracting these phenolic compounds from cereals, using conventional methods, is low, because most of them are bound to the cell wall. Thus, the aim of this study was to optimize the ultrasound‐assisted extraction (UAE) of anthocyanins and total phenolics from sorghum flour, and evaluate the stability of the 3‐DXAs. Two frequencies (25 and 45 kHz) were applied in a Central Composite Rotational design to investigate the effect of the variables time (5–75 min) and temperature (30–65°C) using the UAE, with amplitude of the ultrasonic power set at 400 W. In addition, the stability of the 3‐DXAs present in the extracts was evaluated. It was possible to successfully optimize the extraction of total anthocyanins (both frequencies) and phenolics (at 45 kHz), and then to obtain equations, to predict their concentrations, with high R ² . The efficiency of UAE was observed, increasing the yield of total anthocyanins, phenolics, and antioxidant capacity at the frequencies of 25 and 45 kHz by 30% and 27%, 10% and 5%, and 30% and 15%, respectively. The apigeninidin was the major 3‐DXA found in the extracts, and the luteolinidin was the most stable over storage time. Overall, there was no difference in the 3‐DXAs stability obtained by the UAE compared to the conventional method. Thus, ultrasound is an alternative to obtaining sorghum extracts rich in 3‐DXAs and other phenolic compounds. Practical Application The health benefits of sorghum 3‐deoxyanthocyanins coupled with the growing interest of the food industry in producing healthier food products have motivated this study, because it is important to find ways to optimize 3‐deoxyanthocyanins extraction. We have demonstrated that ultrasound‐assisted extraction was efficient in extracting high amounts of 3‐deoxyanthocyanins and other phenolics from sorghum flour. Moreover, some 3‐deoxyanthocyanins have shown to be more stable than others after extraction. Thus, the ultrasound has great potential to produce sorghum phenolic extracts rich in 3‐deoxyanthocyanins, which can be used as natural colorants and functional ingredients in foods.
Article
In the present study, a medicinal tree named hybrid Eucalyptus was chosen for the extraction of polyphenols from its leaves. Ultrasound has been used for extraction studies, whereas other conventional extraction methods were studied to validate the applied ultrasound assisted extraction method. Various experimental parameters like material to solvent ratio, solvents, and ultrasound irradiation time were employed to obtain the required condition for effective polyphenols extraction. The maximum total polyphenols achieved was 62.24 mg Gallic acid equivalent (GAE)/g of powdered leaves sample with material to solvent ratio of 1:30 and 50% ethanol as solvent with an ultrasonic bath whereas the maximum total flavonoid of 14.20 mg Quercetin equivalent (QE)/g of powdered leaves sample was obtained under the same experimental conditions. The gas chromatography mass spectroscopy (GC‐MS) study of the eucalyptus leaves extract had proved that it contains the required polyphenols of high medicinal value. Also, studies were performed to check 2,2‐diphenylpicrylhydrazyl (DPPH), ferric reducing anti‐oxidant power (FRAP) and 2,2′‐azino‐bis(3‐ethylbenzothiazoline‐6‐sulfonic acid) (ABTS) radical scavenging potential of the leaves extract.
Article
Plants constitute a vital component of the biodiversity as they play a key role in maintaining earth’s environmental equilibrium and ecosystem stability. Herbal medicine is known to be the oldest form of healing, dating back to ancient Greece (1600 BC). It involves the use of plant to improve, maintain or restore health and wholeness. Phytochemicals are bioactive chemicals of plant origin. They are regarded as secondary metabolites synthesized in all parts of the plant body. The quantity and quality of phytochemicals present in plant parts may differ from one part to another. In fact, there is a lack of information on the distribution of the biological activity in different plant parts mainly due to the difference in distribution of active compounds which are more frequent in some plant parts than in others. Colocynthis vulgaris (L) Schrader is one of the medicinal plants of the Cucurbitaceae family, widespread in Algeria mainly in Ouargla in the region of Oued N'sa. This plant is used in traditional medicine for the treatment of several diseases. Its multiple pharmacological properties are due to its richness in active substances, especially alkaloids. The main objective of this study is the comparison between two extraction protocols of alkaloids, one in acid medium and the other in an alkaline medium. The results obtained confirm the plant's richness in alkaloids and the efficiency of the extraction protocol in acid medium.
Thesis
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Phytolacca americana sekonder metabolit
Chapter
Synthetic pigments utilized in food and other allied industries are basically petrochemical-originated chemical dyes. Due to their chemical or petro-originated nature, they impose adverse impacts on human and environment health that drive to accumulate the interest of researchers toward the development of novel, natural, safe, non-toxic, and eco-friendly pigments. This further drives to seek some renewable resources which are not only economical cheaper but also meeting the expectations, to produce the natural pigments. In this regard, the food waste and by-products obtained from the food-processing industries presume immense importance to extract natural pigments as they are an enriched source of natural pigments which can be extracted by employing green extraction technologies or by utilizing the biotechnologically advanced strategies. This chapter entails the various types of natural pigments obtained from food wastes, green extraction technologies, microbial pigments utilizing food wastes, challenges to extraction, and incorporation of the natural pigments in food formulation, stability aspects, and their future prospects. Moreover, the chapter focused on new developments, innovations, and challenges in the extraction of natural pigments directly by using innovative technologies as well as by using microorganisms to exploit their functional potential.
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Bioactive compounds are of considerable interest due to their antioxidant properties and potential beneficial health effects. Thus, this study aimed to optimize and model the ultrasound-assisted extraction process (UAE) of response variables total anthocyanins (TA) and total phenolic content (TPC) from raspberries, and to compare the optimized extraction process with the conventional one. The variables used were time (5 to 75 min), temperature (30 to 70°C), and solid: liquid ratio (1:5 to 1:15 m/v), applied to the Box-Behnken Design (BBD). The optimal condition of the UAE process occurs at a temperature of 70°C and a solid: liquid ratio of 1:12.5 m/v, for both response variables. The optimal time for extraction of TA occurs in 22.5 min predicting the content of 23.181 mg/100 g of the fruit and for TPC occurs in 57.5 min predicting the content of 156.30 mg GAE/100 g of the fruit. On validation of the optimized conditions, less than a 5% difference ware found between the predicted and experimental values (24,131 mg/100 g of fruit for TA, and 149.226 mg GAE/100 g of fruit for TPC). When comparing the optimized UAE with the conventional extraction, it wares observed that UAE increased (p < 0.05) the extraction of TA content by 18.28% and TPC by 28.88%. The process time reduction from 24h in conventional extraction to less than 1h in optimized UAE stands out. Thus, the study indicates that the UAE process is an efficient methodology for recovering bioactive compounds from raspberries.
Article
The growing usage of natural food colourings has fuelled the search for novel methods for their extraction from various sources. Due to its process benefits such as high yield and quality, short extraction periods, use of low temperatures, ultrasound-assisted extraction (UAE) has been studied as a new green strategy. Plant pigments are a rich source of bioactive constituents that could be incorporated in the production of novel functional food additives and an alternative to synthetic substances that can improve the health of consumers. Anthocyanins act as antioxidants, to eliminate the free radicals produced in the body. It is believed that carotenoids offer health benefits through reducing the risk factors associated with certain malignancies and eye diseases. Functions of chlorophyll include aiding in the battle against cancer, facilitating the liver's detoxification process, accelerating the healing of wounds, promoting healthy digestion and weight control, and preserving healthy skin. Betalains contains high soluble fibre content, which effectively lower the levels of LDL cholesterol. In this review, the recent developments about the UAE of various colouring pigments such as anthocyanin, carotenoids, chlorophyll and betalains from different sources and influence of UAE parameters on the extraction yield of colouring pigments were detailed.
Article
Monitoring the characteristic components in tipping paper is important to ensure the quality of cigarette products. This study establishes a method based on gas chromatography (GC) for determining cooling agents in tipping paper. The tipping paper was cut into pieces and extracted by ethanol under specific temperatures in a shaker. Then, the characteristic cooling agents of (-)-menthone, L-menthol, and (-)-menthyl lactate in extract were determined using GC coupled with a flame ionization detector (GC-FID). The limits of detection (LODs) and limits of quantification (LOQs) for the three cooling agents ranged from 0.15~0.32 μg/mL and 0.49~1.06 μg/mL, respectively. Results demonstrated a good linear relationship with high correlation coefficients for the three tested cooling agents. The extraction conditions of the cooling agents were optimized through a single-factor experiment as well as an orthogonal experiment. The standard addition recovery experiment showed that the average recoveries range from 81.23 to 100.62%, and the relative standard deviations (RSDs) of the measured values (n = 5) ranged from 0.34 to 1.64%.
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This work presents the influence of ultrasound pretreatment of Lavandula stoechas on the extraction process of essential oils (EOs), compared with conventional hydrodistillation (HD). This study aims to improve the green techniques for obtaining EOs from aromatic and medicinal plants. The tests were carried out on L. stoechas harvested from 04 sites in the north of Algeria. These samples were pretreated by sonication times of 10, 20, 30, 45 and 60min followed by 90min of HD (US-HD) and compared with untreated samples (180min of HD) in terms of extraction duration, yield, quality, chemical composition and antimicrobial activity of EOs. 10min of pretreatment time gives yields of 1.60% and 1.59% of Kodiat and Adekar EO's, respectively. This pretreatment time proved to be the best compared with the other pretreatment times. The US-HD yields are higher compared to those obtained by HD for the four samples. The US-HD EO's has a darker color and a more intense odor compared with HD EO's. GC/MS analysis showed a qualitative and quantitative difference in the chemical composition of treated and untreated samples. Our extracts showed good antimicrobial activity against most of the 08 pathogenic strains tested. This antimicrobial potential remains more interesting in the US-HD case.
Chapter
Phenolics are some of the most exploited bioactive compounds available in natural resources, attributed to their numerous health benefits, including antioxidant, antidiabetic effects, and effectiveness against neurodegenerative and cardiovascular disorders. Apart from the continual discovery of new original phenolic compounds, researchers have also focused on new analytical and extraction methods to avail easier separation and detection, along with bioavailability studies. Furthermore, recent studies have focused on the discovery and analyses of phenolic composition of nontraditional biological sources, including food industry wastes and agricultural byproducts, with increased emphasis on the valorization of waste. Interest in this regard has also encouraged the novel applications of these extracted biomolecules in food, feed, and nutraceutical developments along with other applications, such as storage life and quality enhancers for various products. Hence, this chapter has summarized the recent topics of interest in this field along with an update regarding the applications of traditional techniques, focusing on the novel techniques employed for the identification of these compounds, along with pioneering and advanced analytical and extraction/separation methods specifically developed, as well as used in the studies of phenolic compounds. Factors affecting the preharvest accumulation and postharvest enhancement of the concentrations of these compounds in the biological material have also been briefly discussed. New applications and potential future trends in the research on phenolic compounds have also been briefly discussed.
Thesis
Tez bitkilerde koruma,savunma ve üreme gibi fonksiyonları olan aynı zamanda ilaç yapımı, kozmetik gibi birçok alanda kullanılan sekonder metabolitler üzerinedir.
Chapter
This chapter provides insight into the basics concepts in the analysis of phenolic compounds. The extraction of phenolic compounds is carried out using ultrasound-assisted, microwave-assisted, ultrasound/microwave-assisted, ultrasound-assisted enzymatic, microwave-assisted enzymatic, supercritical fluid, subcritical water, high hydrostatic pressure, and cyclodextrin-assisted extraction processes. The analytical methodologies for the determination of phenolic compounds using several spectrophotometric methods, potentiometric, and electrochemical methods have been discussed in detail.
Conference Paper
Polyphenols as phytochemicals are found abundantly in plant matrices. Recently, the importance of polyphenols has increased worldwide owing to different health benefits and therapeutic advantages associated with polyphenols in order to mitigate the lifestyle disorders and oxidative stress to improve the overall human wellness. Conventional extraction methods have been in place for centuries for extraction of polyphenols. These conventional methods exhibit several inherent limitations, and to date, efficient, rapid and clean recovery of polyphenols has remained a challenging task by developing a single standard and optimized method. Based on greener approach, the exploitation of phenolic compounds as supplements and natural antioxidants on commercial scale has escalated the exploration efforts for cost-effective, efficient and eco-friendly extraction methods. In this overview, updated technical information regarding modern extraction techniques, such as supercritical fluid extraction, ultrasound-assisted extraction, microwave-assisted extraction, pressurized liquid extraction, and pressurized hot water extraction–as green alternatives to conventional extraction methods– was presented along with their advantages, disadvantages, factors governing extractions mechanisms and applications with regard to green extraction of phenolic compounds from plants matrices. Furthermore, prominent advantages offered by modern extraction techniques comprise of reduced solvent and time consumption with considerably lower operational costs by virtue of overcoming limitations of conventional extraction for polyphenol extraction. Further research is a need of time to investigate the mechanisms underpinning the extraction kinetics of green methods to scale up on an industrial scale for extracting polyphenols from plant matrices. The challenges faced by the 21st century can be met by provision of protection to both environment and consumers and food industries are evolving by competing to combat these challenges keeping in view the eco-friendly and economic niches. This green approach ranges from harvesting and production stages and encompasses the transformation of the separation and extraction processes in conjunction with formulations and marketing. These green extracts would be identified in future with pertinent label as per the European and international regulations.
Conference Paper
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عصاره¬های گیاهی به طور وسیعی در صنایع دارویی، غذایی و بهداشتی مورد استفاده قرار می¬گیرند، فناوري¬هاي عصاره¬گیري مختلفی وجود دارند که می¬توانند این ترکیبات فعال را از منابع گیاهی استخراج نمایند. روش¬هاي سنتی استخراج نظیر روش غرقابی و سوکسله نیاز به صرف زمان طولانی و مقدار حلال زیاد دارند همچنین از لحاظ دمایی ایمن نیستند و باعث تجزیه تعدادي از ترکیبات می¬شوند. به همین دلیل تقاضاي زیادي براي روش¬هاي عصاره¬گیري جدید با زمان کوتاه¬تر، میزان مصرف حلال کمتر و محافظ محیط زیست وجود دارد. در این مقاله به معرفی بیشتر فراصوت به عنوان یکی از روش¬های نوین در استخراج ترکیبات طبیعی گیاهان پرداخته می¬شود که نسبت به روش¬هاي متداول، كارايي بالاتر، كاهش زمان عصاره¬گيري و كاهش مصرف حلال را به دنبال داشته است.
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Twenty colonies of Pediococcus acidilactici, Lactobacillus brevis, Lactiplantibacillus plantarum and Latilactobacillus curvatus were isolated from fermentation broth of pickled pepper by using MRS agar. The strains were acclimated using high pressure from 300 to 400 MPa for 1 to 5 min. For one generation of acclimation, the survived cells after first high pressure treatment were then activated by culturing on MRS agar for two days for the next high pressure treatment. After acclimation for 30 generations, the survival ratio of L. plantarum and L. curvatus was increased by 138 and 1222 times at 400 MPa for 1 and 3 min, respectively. Weibull model could appropriately fit the survival curves of L. plantarum and L. curvatus treated by high pressure. The time to the first decimal reduction of these two strains after acclimation was 3.5 and 1.8 times, respectively, longer than before acclimation at 300 MPa. From electron microscopy photographs, the acclimated L. curvatus was more curved, smaller and its cell wall was thicker than the unacclimated L. curvatus. After HPP treatment, L. plantarum and L. curvatus have higher cell integrity, smoother cell surface, more uniform protoplasm and smaller cavities in the cell protoplasm compared with unacclimated strains, suggesting that high pressure acclimation introduced some modification to bacteria intrinsic structures and increased their pressure resistance. Moreover, the fermentation performance including glucose utilization capacity and lactic acid production of the acclimated L. curvatus was respectively improved by 9.6% and 9.4% at 37 °C for 24 h in MRS medium.
Article
The selection of appropriate conditions for increasing the extraction efficiency is important. The response surface method (RSM) is a statistical and mathematical technique which it can be used to examine the dependence between the responses with variables in a process and also determine the optimal conditions. In this study, the experimental design of General full factorial (GFF) was used by Minitab 17 software. The variables were time (30, 60 and 90 min), solvent (water, methanol and n-hexane) and method (maceration and ultrasound-assisted extraction). The main effects and also interaction terms were investigated on amounts of total phenolic content (TPC), total flavonoid content (TFC) and the antioxidant activity (according to DPPH, FRAP, IC50 and BCB) of extract of Arenaria hispanica L.. A multiple regression, first degree model was used to express the responses. An analysis of variance (ANOVA) with 95% confidence level was then carried out for each response (TPC, TFC, FRAP, IC50 and BCB) in order to test the model significance and suitability. In optimum conditions, the maceration method was optimum method for TPC, FRAP and BCB, while for TFC was ultrasound-assisted extraction. Water was optimal solvent for TPC, FRAP and BCB, but methanol was obtained as the best solvent for TFC and IC50. Also, the extraction time of TPC was 60 min and for TFC, IC50, FRAP and BCB obtained 30 min. The mounts of TPC, TFC, IC50, FRAP and BCB in the optimum conditions obtained 173.93 ± 0.50 (mg GAE/g extract), 184.27 ± 4.04 (mg QC/g extract), 0.69 ± 0.03 (mg/mL), 734.80 ± 2.02 (mmol Fe2+/g exctract) and 21.23 ± 0.22; respectively.
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Using a continuous decorticating machine, white dent corn was efficiently separated, after brief steeping in water, into two fractions: the first (12.5%) consisting mainly of pericarp, germ, and tip cap (PGT); the second (87.5%) consisting of endosperm. Nixtamalization of the maize fractions in the presence of 0.6% (w/w) lime caused an increase in the hot-paste viscosity at 90degreesC, while nixtamalization of PGT at lime inputs <0.6% (w/w) resulted in decreased viscosity. Three domains were found for the viscosity of nixtamalized endosperm at 90degreesC: lower concentrations of lime (<0.15%, w/w) resulted in lower viscosity values; increased lime (0.15% - <0.3%, w/w) increased the viscosity values; and a lime concentration of 0.3% (w/w) resulted in a lower viscosity value. The response variables (water absorption index, water solubility index, initial viscosity, and viscosity at 90degreesC for nixtamalized PGT, and compression force and compression area of tortillas) indicated that the mathematical models fit the experimental data and the variance of the models was highly significant. Tortillas of good functional characteristics similar to tortillas produced by the traditional process were obtained when 5% nixtamalized fractions of PGT were blended with 95% nixtamalized endosperm.
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Ample research indicates that age-related neuronal-behavioral decrements are the result of oxidative stress that may be ameliorated by antioxidants. Our previous study had shown that rats given dietary supplements of fruit and vegetable extracts with high antioxidant activity for 8 months beginning at 6 months of age retarded age-related declines in neuronal and cognitive function. The present study showed that such supplements (strawberry, spinach, or blueberry at 14.8, 9.1, or 18.6 gm of dried aqueous extract per kilogram of diet, respectively) fed for 8 weeks to 19-month-old Fischer 344 rats were also effective in reversing age-related deficits in several neuronal and behavioral parameters including: oxotremorine enhancement of K(+)-evoked release of dopamine from striatal slices, carbachol-stimulated GTPase activity, striatal Ca(45) buffering in striatal synaptosomes, motor behavioral performance on the rod walking and accelerod tasks, and Morris water maze performance. These findings suggest that, in addition to their known beneficial effects on cancer and heart disease, phytochemicals present in antioxidant-rich foods may be beneficial in reversing the course of neuronal and behavioral aging.
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The sonolysis of water and some organic liquids such as ethylene glycol, methanol and chloroform in the presence of oxygen, at 20 and 475 kHz ultrasound frequencies has been investigated by the ESR-spin trapping technique. 5,5-Dimethyl-1-pyrroline-N-oxide (DMPO), 3,3,5,5-tetramethylpyrroline-N-oxide (TMPO) and N-tert-butyl-alpha-phenyl nitrone (PBN) were able to trap superoxide radical anion, generated as the result of the sonication of the organic media. The addition of superoxide dismutase (SOD) resulted in a dramatic decrease of the ESR signal intensity of the superoxide radical adduct. In addition, the thermolysis of the liquids under ultrasound was shown by ESR detection of the spin adducts of the radicals formed by homolytic fragmentation. Occasionally, the nature of the detected spin adduct was dependent on the sonication time or on the frequency of the ultrasonic radiation. Experiments carried out in the presence of 2-methyl-2-nitrosopropane (MNP) resulted in the detection of radicals originating from thermal decomposition of the spin trap, showing its lability under ultrasonic radiation.
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Ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction methods for the isolation of ginsenosides (saponins) from various types of ginseng. The ginseng samples were extracted with different solvents, under either direct sonication by an ultrasound probe horn or indirect sonication in an ultrasound cleaning bath. The ultrasonic extraction was compared with the conventional method of refluxing boiling solvents in a soxhlet extractor, on the yields of both the total saponin isolated by thin-layer chromatography and the individual ginsenosides by high performance liquid chromatography. It was found that the sonication-assisted extraction of ginseng saponins was about three times faster than the traditional extraction method. The ultrasonic extraction was not only more efficient but also convenient for the recovery and purification of the active ingredients of plant materials. In addition, the sonication-assisted extraction can be carried out at lower temperatures which are favorable for the thermally unstable compounds.
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The following four methods were compared on the extraction efficiency of 16 EPA (US Environmental Protection Agency) polycyclic aromatic hydrocarbons (PAHs): German method of the Verband Deutscher Landwirtschaftlicher Untersuchungs und Forschungsanstalten (VDLUFA), two methods of the International Organization for Standardization using shaking (ISO A) and Soxhlet extraction (ISO B) and an ultrasonic method. Recovery rates of 16 PAHs were determined in two soils. Extraction efficiency was evaluated in five soils and three sediments. Effect of drying soils and sediments on extraction efficiency was tested using the VDLUFA and the ultrasonic methods. Our study shows that the number of aromatic rings, rather than extraction procedures, significantly influenced recovery rates of individual PAHs. No significant differences in extraction efficiency of the four methods were observed for less polluted samples. For highly polluted soils, extraction efficiency decreased in the following order: VDLUFA method > ISO A > ultrasonic method > ISO B. Influence of soil moisture on extraction efficiency depended to some extent on both solvent used and content of PAHs in samples. A mixture of dichloromethane/acetone (5:1) is recommended for PAH extraction from moist samples when the ultrasonic method is used.
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Fricke reaction, KI oxidation and decomposition of porphyrin derivatives by use of seven types of sonochemical apparatus in four different laboratories were examined in the range of frequency of 19.5 kHz to 1.2 MHz. The ultrasonic energy dissipated into an apparatus was determined also by calorimetry. Sonochemical efficiency of Fricke reaction and KI oxidation was defined as the number of reacted molecule per unit ultrasonic energy. The sonochemical efficiency is independent of experimental conditions such as the shape of sample cell and irradiation instruments, but depends on the ultrasonic frequency. We propose the KI oxidation dosimetry using 0.1 moldm(-3) KI solution as a standard method to calibrate the sonochemical efficiency of an individual reaction system.
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In the high technology arena, increasing importance is placed on effective management of new technology introduction, from the conceptual phase through laboratory testing and transition to production. Advances in Information Technology that include both hardware and software have brought simulation capabilities to desktop computers. American Technology & Services (ATS), a leader in manufacturing cost estimating and modeling has developed a technique of Manufacturing Process Flow Simulation (MPFS) for analyzing the economics of manufacturing processes. The capabilities of this technique will be illustrated by an example of a simulation model based on the manufacturing of a high temperature (232 - 371 °C) Organic Matrix Composite (OMC) - an advanced material for which little historical cost data is available. Observations resulting from this analysis include process metrics such as cycle time, process capacity, and the early identification of bottlenecks or other resource related problems early in the design cycle. In conclusion, the MPFS cost model provides design engineers and management the capability of analyzing the manufacturing environment as a dynamic system. This permits up-front development of the process rather than problem solving after the fact and will result in implementation of an `optimized' process, under-budget and on-schedule.
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SUMMARY— The method developed consists of extracting the anthocyanins with ethanol-1.5N hydrochloric acid (85:15) and measuring the O.D. of the extract, diluted with the extracting solvent, at 535 nm. The total anthocyanin content was calculated in absolute quantities with the aid of the extinction coefficients established for the four major cranberry anthocyanins dissolved in the alcoholic solvent system.
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Suppose that a relationship $\eta = \varphi(\xi_1, \xi_2, \cdots, \xi_k)$ exists between a response $\eta$ and the levels $\xi_1, \xi_2, \cdots, \xi_k$ of $k$ quantitative variables or factors, and that nothing is assumed about the function $\varphi$ except that, within a limited region of immediate interest in the space of the variables, it can be adequately represented by a polynomial of degree $d$. A $k$-dimensional experimental design of order $d$ is a set of $N$ points in the $k$-dimensional space of the variables so chosen that, using the data generated by making one observation at each of the points, all the coefficients in the $d$th degree polynomial can be estimated. The problem of selecting practically useful designs is discussed, and in this connection the concept of the variance function for an experimental design is introduced. Reasons are advanced for preferring designs having a "spherical" or nearly "spherical" variance function. Such designs insure that the estimated response has a constant variance at all points which are the same distance from the center of the design. Designs having this property are called rotatable designs. When such arrangements are submitted to rotation about the fixed center, the variances and covariances of the estimated coefficients in the fitted series remain constant. Rotatable designs having satisfactory variance functions are given for $d = 1, 2$; and $k = 2, 3, \cdots, \infty$. Blocking arrangements are derived. The simplification in the form of the confidence region for a stationary point resulting from the use of a second order rotatable design is discussed.
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The Galvani potential has been used to study the removal of solder flux from electronic circuit boards with and without ultrasound. First a theory of the Galvani potential as applied to decontamination studies is presented. Then theoretical decontamination curves are presented, based on simple chemical kinetics coupled to mass diffusion to and from the surface through a passive boundary layer. Finally, the theory is tested and illustrated by removal of solder flux from finger structures in various solvents including freon, Prelete, and isopropanol in water. Clear differences in how quickly the Galvani potential decreased with time were noted. The fastest results were obtained for 80% isopropanol in water, but it is likely that more metallic salts were left behind on the surface than in the slower methods. The saturation of the solvents is also discussed. Finally, methods of on-line testing solvents and circuit boards based on the Galvani potential are discussed.
Article
The goal of this study was to determine the efficacy of ultrasonication extraction of 1,1,1-trichloro-2,2-bis[p-chlorophenyl]ethane (DDT), 1,1-dichloro-2,2-bis[p-chlorophenyl]ethane (DDD), and 2,2-bis[p-chlorophenyl]1,1-dichloro-ethylene (DDE) residues in soil for the purposes of saving time, minimizing generation of hazardous solvent wastes, and reducing costs associated with monitoring contaminant concentrations at remediation sites. An ultrasonic extraction method was developed for DDT, DDD, and DDE residues in soil, and the efficiency of extraction using an ultrasonic cavitator was compared to the traditional soxhlet method by GC-MS. Un-contaminated soil was spiked with analytes DDT, DDD, and DDE at 0.1,1.0,10.0, and 100.0 mg/ kg. Experiments were performed in triplicate, and recoveries of analytes were determined and statistically compared. Results indicate that ultrasonic extraction is a suitable preparatory method for analysis of DDT, DDD, and DDE residues in soil. For spike concentrations of 1 mg/kg to 100 mg/kg, ultrasonication extraction resulted in recoveries in excess of 80% in all but one case. Most recoveries obtained by ultrasonication extraction were statistically indistinguishable from or slightly lower than recoveries obtained by soxhlet extraction. In addition, the lower temperatures employed in ultrasonication extraction may have reduced the amount of thermal degradation of DDT to DDE, a phenomenon that could occur during soxhlet extraction.
Article
The effect of ultrasound- and microwave-assistance in enhancing extraction oil yields from soybeans when different solvents are used for extraction was investigated in two separate experiments. Each study involved a three-factor factorial following a completely randomized design that was replicated three times. Treatment factors investigated in the microwave processing study were microwave pretreatment time (0, 0.5, 1, and 2 min), solvent (isopropanol, hexane, 3:2 hexaneisopropanol mixture), and extraction time (0.5, 1, 1.5, 2, and 3 h). Ultrasonic intensity (0, 16.4, 20.9, and 47.6 W/cm2) was substituted as a treatment factor in the sonication study. Solvent extraction was accomplished by immersion of ground soybeans in a given volume of solvent at ambient temperature. While oil yields did not approach the 19.2% analyzed oil content of the TN 96-58 used as the test material, they were found to increase with both intensity of the process assistance and extraction time under the conditions of the studies particularly with hexane and the mixed solvent. The highest yield result of 12.21 g from 100 g soybeans was obtained with the mixed solvent under 47.6 W/cm2 sonication. The results obtained with the mixed solvent with both microwave pretreatment and ultrasound assistance are difficult to explain in terms of physical chemistry. The results with isopropanol indicate that the efficiency of the extraction process depends greatly on the molecular affinity between solvent and solute and that process assistance tested in this study cannot overcome inherent deficiencies in solvent-solute interactions.
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Sonochemistry is the use of ultrasound to enhance or alter chemical reactions. Sonochemistry in the true sense of the term occurs when ultrasound induces “true” chemical effects on the reaction system, such as forming free radicals which accelerate the reaction. However, ultrasound may have other mechanical effects on the reaction, such as increasing the surface area between the reactants, accelerating dissolution, and/or renewing the surface of a solid reactant or catalyst. This comprehensive review summarizes several topics of study in the sonochemical literature, including bubble dynamics, factors affecting cavitation, the effects of ultrasound on a variety of chemical systems, modeling of kinetic and mass-transfer effects, the methods used to produce ultrasound, proposed cavitation reactors, and the problems of scaleup. The objective of this paper is to present a critical review of information available in the literature so as to facilitate and inspire future research in the field of sonochemistry.
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The anthocyanin and flavonol pigments of the miracle fruit (Synsepalum dulcificum, Schum) were isolated and identified by paper chromatography and spectral analysis. The red pigments of miracle fruit (14.3 mg/100g fresh wt) were cyanidin-3-monogalactoside, cyanidin-3-monoglucoside, cyanidin-3-monoarabinoside, delphinidin-3-monogalactoside and delphmidin-3-monoarabinoside existing in a ratio of 188:62:9:5:2, respectively. The major flavonol pigments were quercetin-3-monogalactoside, kaempferol-3-monoglucoside, myricetin-3-monogatactoside and traces of similar flavonols. The aglycones quercetin, kaempferol and myricetin were also isolated and identified. The flavonols and aglycones were present at 9.0 mg/100g fresh wt.
Article
SUMMARY— The evaluation of the various purification methods was based, in the order of their importance, on the recovery of individual and total anthocyanins and on the concentrating power. Amberlite CG-50 ion exchange resin was the best, but basic lead acetate was also satisfactory. Polyamide did not concentrate the anthocyanins and the use of neutral lead acetate resulted in poor recoveries.
Article
The use of manothermosonication (MTS), a combined treatment of heat and ultrasound (20 kHz frequency) under moderate pressure, has been recently proposed as an alternative to conventional heat treatment of liquid foods. The efficiency of MTS has been proved on several enzymes of interest in food industry. One of the MTS enzyme inactivation mechanisms proposed is the interaction of free radicals produced by water sonolysis with some amino acid residues. In this paper we examine the rate of free radical production of the MTS system under different conditions of temperature, pressure and ultrasound amplitude using the terephtalate dosimeter.The ultrasound amplitude was varied between 20 and 145 μm at two different temperatures and pressures ( and ). In both cases, free radical production rate increases linearly with increasing ultrasound amplitude.The pressure effects on free radical production was studied under two different conditions at 117 μm: 70 °C and 130 °C. At 70 °C an increase of hydrostatic pressure results in an increase in free radical production rate, whereas increasing hydrostatic pressure at 130 °C had a negligible effect on free radical production rate.Temperature effects were studied between 30 and 140 °C at 117 μm ultrasound amplitude. Results show that increasing temperature results in a decrease in hydroxyl radical rate production.
Article
Ultrasonic solvent extraction of the pesticides atrazine, propham, chlorpropham, diflubenzuron, α-cypermethrin and tetramethrin from soil is reported. The extraction procedure was optimized with regard to the amount of solvent, the duration of sonication and the number of extraction steps. Ultrasonic solvent extraction was compared with traditional extraction methods, shake-flask and Soxhlet extraction. The recovery of pesticides was determined by quantitative thin-layer chromatography on RP-18 plates. Ultrasonic extraction using acetone showed satisfactory extraction efficiencies combined with simplicity of use and low solvent consumption.
Article
By-products obtained after red fruit processing still contain large amounts of polyphenols, especially anthocyanins which act as antioxidants. The effect of solvent and extraction time on the yield of extracted antioxidants from grape, black and red currant by-products (marc) was investigated. Ethanol and methanol extracts of red and black currant contain twice more anthocyanins and polyphenols than water extracts, extracts made from grape marc had seven times higher values than water extracts. In water extracts the yields of polyphenols decreased, while in methanol and ethanol extracts their content increased with the time of extraction. The highest antioxidant activity was in extracts made from black currant marc, the lowest was in extracts made from red currant marc. Grape extracts had high antioxidant activity due to its high content of polyphenols.
Article
The application of 20 kHz high-intensity ultrasound during extraction of oil from two varieties of soybeans (TN 96-58 and N 98-4573) using hexane, isopropanol and a 3:2 hexane–isopropanol mixture was evaluated. In a simplified extraction procedure, ground soybeans were added to solvents and ultrasonicated between 0 and 3 h at ultrasonic intensity levels ranging from 16.4 to 47.6 W/cm2. Oil was recovered after distillation and yield and composition determined. Using hexane as a solvent, yield generally increased as both application time and intensity of ultrasound increased. Solvent type influenced the efficiency of the extraction, i.e., the highest yield was obtained using ultrasound in combination with the mixed solvent. Gas chromatography analysis of ultrasonicated soybean oil did not show significant changes in fatty acid composition. Results were attributed to mechanical effects due to ultrasonically induced cavitation increasing permeability of plant tissues. A comparison of scanning electron microscopy images of raw and ultrasonicated soybeans indicated development of microfractures and disruption of cell walls in ground soybean flakes. Our study suggests that high-intensity ultrasound may reduce time required to extract edible oils from plant sources and hence improve throughput in commercial oil production processes.
Article
In recent years, microwave-assisted extraction has attracted growing interest as it allows rapid extractions of solutes from solid matrices, with extraction efficiency comparable to that of the classical techniques. In particular, numerous applications of this recent technique deal with the extraction of pollutants from environmental samples. This review gives a brief presentation of the theory of microwave and extraction systems, a discussion of the main parameters that influence the efficiency, and the main results on the applications to environmental matrices. Finally, the performance of this technique is compared to that from classical extractions (sonication and Soxhlet extraction) and recent techniques (supercritical fluid extraction and accelerated solvent extraction).
Article
Studies of distribution, extraction procedures and spiking protocols in the determination of incurred chloramphenicol residues in animal tissues have been carried out. An extraction procedure involving glucuronidase enzyme digestion was found to extract 10 times more incurred chloramphenicol from pig kidney than direct extraction without digestion. However, neither protease digestion nor ultrasonic probe treatment resulted in improved chloramphenicol extraction. Chloramphenicol was found to be inhomogeneously distributed within kidney from a treated pig. Highest concentrations were detected in the renal medulla. Muscle tissues from the same animal were found to contain a lower concentration of chloramphenicol residues, but no chloramphenicol residues were detectable in the liver. Chloramphenicol recovery from spiked pig liver was found to be lower than that from kidney, but was improved by the addition of piperonyl butoxide before extraction. This additive had no effect on recovery from spiked pig or cattle kidney. The implications of these results for regulatory surveillance of animal tissue for chloramphenicol residues are discussed.
Article
Because contaminants in recycled paper intended for food packaging could be a risk to public health, analytical methods are needed to identify and quantify residues of concern in paper/paperboard. The U. S. Food and Drug Administration is considering development of a guidance document for testing levels of contaminants that might be retained through paper recycling processes. An analytical procedure was developed using paper spiked with suspected contaminants at concentrations of 1-50 ppm in the paper. Benzophenone, dimethyl phthalate, anthracene, methyl stearate, and pentachlorophenol were introduced by soaking the paper in a solution in acetone at 25 degrees C for 24 h; the paper was removed and dried by evaporating the solvent with nitrogen. The model contaminant residues were extracted from the paper using ultrasonication and quantified by GC with flame ionization and electron capture detectors. Recoveries from the spiked paper were 80-109% with a repeatability of +/-4%. The method was also used to analyze commercial recycled paperboard to validate its applicability.
Article
A method has been established and validated for identification and quantification of individual, as well as total, anthocyanins by HPLC and LC/ES-MS in botanical raw materials used in the herbal supplement industry. The anthocyanins were separated and identified on the basis of their respective M(+) (cation) using LC/ES-MS. Separated anthocyanins were individually calculated against one commercially available anthocyanin external standard (cyanidin-3-glucoside chloride) and expressed as its equivalents. Amounts of each anthocyanin calculated as external standard equivalent were then multiplied by a molecular-weight correction factor to afford their specific quantities. Experimental procedures and use of a molecular-weight correction factors are substantiated and validated using Balaton tart cherry and elderberry as templates. Cyanidin-3-glucoside chloride has been widely used in the botanical industry to calculate total anthocyanins. In our studies on tart cherry and elderberry, its use as external standard followed by use of molecular-weight correction factors should provide relatively accurate results for total anthocyanins, because of the presence of cyanidin as their major anthocyanidin backbone. The method proposed here is simple and has a direct sample preparation procedure without any solid-phase extraction. It enables selection and use of commercially available anthocyanins as external standards for quantification of specific anthocyanins in the sample matrix irrespective of their commercial availability as analytical standards. It can be used as a template and applied for similar quantification in several anthocyanin-containing raw materials for routine quality control procedures, thus providing consistency in analytical testing of botanical raw materials used for manufacturing efficacious and true-to-the-label nutritional supplements.
Article
Analysis of extracts of Glen Ample raspberries (Rubus idaeus L.) by gradient, reverse phase HPLC with diode array and tandem mass spectrometry identified eleven anthocyanins, including cyanidin-3-sophoroside, cyanidin-3-(2(G)-glucosylrutinoside), cyanidin-3-glucoside, cyanidin-3-rutinoside, pelargonidin-3-sophoroside, pelargonidin-3-(2(G)-glucosylrutinoside), and pelargonidin-3-glucoside. Significant quantities of an ellagitannin, sanguiin H-6, with an M(r) of 1870 were detected along with lower levels of a second ellagitannin, lambertianin C, which has an M(r) of 2804. Other phenolic compounds that were detected included trace levels of ellagic acid and its sugar conjugates along with one kaempferol- and four quercetin-based flavonol conjugates. Fractionation by preparative HPLC revealed that sanguiin H-6 was a major contributor to the antioxidant capacity of raspberries together with vitamin C and the anthocyanins. Vasodilation activity was restricted to fractions containing lambertianin C and sanguiin H-6.
Article
Anthocyanins from red raspberries were extracted from the fruit by homogenizing in acidified methanol. The methanolic extract was centrifuged and the supernatant analyzed by reversed-phase HPLC. The eluent was monitored at 371 and 520 nm before being introduced into a single quadrupole mass spectrometer through an atmospheric pressure chemical ionization probe operating in positive ion mode. This method allowed the identification of eight anthocyanins. In the absence of readily available reference compounds, approaches that can be taken to analyse anthocyanins by HPLC with absorbance and mass spectrometric detection are discussed.
Article
The effects of elevated CO2 concentrations on the antioxidant capacity and flavonoid content in strawberry fruit (Fragaria x ananassa Duch.) were studied under field conditions. Increased CO(2) (300 and 600 micromol mol(-1) above ambient) concentrations resulted in increases in ascorbic acid (AsA), glutathione (GSH), and ratios of AsA to dehydroascorbic acid (DHAsA) and GSH to oxidized glutathione (GSSG), and a decrease in DHAsA in strawberry fruit. High anthocyanin and phenolic content were also found in fruit of CO(2) treated plants. Growing strawberry plants under CO(2) enrichment conditions significantly enhanced fruit p-coumaroylglucose, dihydroflavonol, quercetin 3-glucoside, quercetin 3-glucuronide, and kaempferol 3-glucoside contents, as well as cyanidin 3-glucoside, pelargonidin 3-glucoside, and pelargonidin 3-glucoside-succinate content. Fruit of strawberry plants grown in the CO(2) enrichment conditions also had high oxygen radical absorbance activity against ROO(*), O(2)(*-), H(2)O(2), OH(*), and (1)O(2) radicals.
Article
Efficiency in extracting four isoflavone derivatives (daidzin, glycitin, genistin and malonyl genistin) from freeze-dried ground soybeans was compared for mix-stirring extraction and ultrasound-assisted extraction, using different solvents and extraction temperatures with both. The efficiency of the extraction of soy isoflavones was improved by ultrasound but was dependent on the solvent employed. Optimization of the ratios of sample quantity to solvent volume and length of extraction time was also performed. Isoflavones can be quantitatively extracted from soybeans with 50% ethanol at 60 degrees C using ultrasound-assisted extraction in 20 min.
Article
Anthocyanins are naturally occurring compounds that impart color to fruits, vegetables, and plants. They are probably the most important group of visible plant pigments besides chlorophyll. Apart from imparting color to plants, anthocyanins also have an array of health-promoting benefits, as they can protect against a variety of oxidants through a various number of mechanisms. However, anthocyanins have received less attention than other flavonoids, despite this. This article reviews their biological functions and pre-clinical studies, as well as the most recent analytical techniques concerning anthocyanin isolation and identification.
Article
Anthocyanins and phenolics of 10 blue honeysuckle (Lonicera caerulea L.) genotypes were characterized and quantified by HPLC-DAD. Peak assignments were confirmed by low-resolution electrospray mass spectrometry. Six anthocyanins were detected with the major peak identified as cyanidin 3-glucoside. Five additional anthocyanins were characterized as cyanidin 3,5-diglucoside, cyanidin 3-rutinoside, pelargonidin 3-glucoside, peonidin 3-glucoside, and peonidin 3-rutinoside. Four polyphenolics were identified as chlorogenic acid, neochlorogenic acid, quercetin 3-rutinoside, and quercetin 3-glucoside. Two additional unidentified phenolics were characterized as flavonol and hydroxycinnamic derivatives based on UV-vis spectra. Hydroxycinnamate levels ranged from 30.4 to 156.2 mg/100 g, whereas the flavonol content ranged from 12.6 to 32.8 mg/100 g. The L. caerulea subspecies boczkarnikovae contained the highest amounts of hydroxycinnamic derivatives and flavonols.
Article
This work examines the concurrent use of power ultrasound during the extraction of pungent compounds from a typical herb (ginger) with supercritical CO(2). A power ultrasonic transducer with an operating frequency of 20 kHz is connected to an extraction vessel and the extraction of gingerols from freeze-dried ginger particles (4-8 mm) is monitored. In the presence of ultrasound, we find that both the extraction rate and the yield increase. The higher extraction rate is attributed to disruption of the cell structures and an increase in the accessibility of the solvent to the internal particle structure, which enhances the intra-particle diffusivity. While cavitation would readily account for such enhancement in ambient processes, the absence of phase boundaries should exclude such phenomena above the critical point. Possible alternate mechanisms for the cell structure damage are discussed.
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7. HPLC profile of anthocyanin extract by UAE and conventional extraction
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Fig. 7. HPLC profile of anthocyanin extract by UAE and conventional extraction.
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