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Ultrasound-assisted extraction of D-pinitol from carob pods using Response Surface Methodology

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... carob and Soya beans. Not only ultrasound assisted extraction was more efficient in D-pinitol extraction than conventional hot water but also in lowering extraction temperature, time as well as energy consumption (Tetik and Yüksel 2014). ...
... In traditional medicine, brewer of carob powder is recommended as an anti-diarrheal remedy especially for infants (Loeb et al. 1989). Carob soft drink is particularly effective for the treatment of GIT disorders asides from a mild diuretic action based on its richness in minerals and electrolytes (Tetik and Yüksel 2014). Traditional uses of pods include their application as an anti-tussive agents and against heartburn and warts (Amico and Sorce 1997). ...
... Secondary metabolite profiles of carob extracts comprise several types of gallic acid conjugates, condensed tannins and other phenolic compounds imposing an astringent and anti-microbial effects, a prerequisite for the control of diarrhea (Avallone et al. 1997;Tetik and Yüksel 2014;Hsouna et al. 2011;Papagiannopoulos et al. 2004). A dietary preparation of carob pods particulate, containing at least 20%, of water-insoluble tannins by weight is patented in the US for the treatment of diarrhea (Wursch 1991). ...
Chapter
Ceratonia siliqua (Carob); is a Mediterranean legume globally recognized for its commercial value, being used as a cold beverage, in bakery and confectionary products. It is widely used as a Cocoa substitute not only due to its richness in sugar but rather the absence of caffeine and theobromine stimulant action. Both fruit pulp and seeds are of potential nutritive and medicinal values. The pulp comprises a high sugar content dominantly sucrose as well as polyphenols viz. phenolic acids, flavonoids and tannins. Seeds potential usage is attributed to its locust bean gum (LBG), commercially and pharmaceutically used as gelling and stiffening agent. Carob syrup is a traditional product native to the Mediterranean region, enriched in D-pinitol sugar of anti-diabetic effect. Considering the diversity of carob active constituents’ classes, a myriad of biological effects is recorded to include antioxidant, anticancer, antimicrobial and anti-hyperlipidemic effects. This book chapter presents up to date information on carob usage and chemistry while providing insight on research questions or applications yet to be addressed.
... It was first isolated in the sugar pine (Pinus Lambertiana) (Anderson et al., 1952). D-pinitol is a naturally occurring compound present in peanut (Lee and Morris, 1963), Bougainvillea spectabilis (Jawla et al., 2013;Narayanan et al., 1987;Vidhate et al., 2015), and Argyrolobium roseum (Ram et al., 2007;Sharma et al., 2016), but for manufacturing purposes it is generally extracted from soybean (Kawai and Kumazawa, 1982;Phillips et al., 1982;Streeter et al., 2001) and also from carob (Baumgartner et al., 1986;Cháfer and Berna, 2014;Tetik and Yüksel, 2014). ...
... Bubbles can help in the disruption of plant cell wall and enhance penetration of the solvent into the plant cell, which results in greater extraction yield of bioactive compounds. There are several reports describing the use of ultrasound for extraction of cyclitols from plants ( Gómez-González et al., 2010;Tetik and Yüksel, 2014). Tetik and Yüksel (2014) studied extraction efficiency of D-pinitol from carob pods using UAE with varying parameters such as temperature, ultrasonic power, dilution rate (material: water ratio) and time. ...
... There are several reports describing the use of ultrasound for extraction of cyclitols from plants ( Gómez-González et al., 2010;Tetik and Yüksel, 2014). Tetik and Yüksel (2014) studied extraction efficiency of D-pinitol from carob pods using UAE with varying parameters such as temperature, ultrasonic power, dilution rate (material: water ratio) and time. The authors report that the highest concentration of D-pinitol (11.98 g/L) was obtained by using the following parameters: temperature 50 C, ultrasonic power 207 W, dilution rate of 1:4 and extraction time 120 min. ...
Article
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Cyclitols are cycloalkanes with one hydroxyl group on each of three or more ring atoms, also called cycloalkane polyols or sugar alcohol which attract attention since they have numerous pharmaceutical properties and are widespread in the plants. Inositols are important cyclitols, which constitute a group of naturally occurring polyhydric alcohols and some isomers of this group can be commonly found in most plants, provided adequate methods of detection are employed. This review presents plant containing cyclitols, with emphasis put on their pharmaceutical properties. The text focuses on sample preparation, extraction and purification and on analysis of cyclitols in plants. In addition, it addresses the application of different methodologies utilized in the analysis of cyclitol compounds in plant.
... The efficiency of UAE is generally influenced by several factors, including solvent-solid ratio, solvent type and concentration, particle size, and extraction time and temperature [17]. Many researches have shown that the highest extraction of polyphenols and other bioactive compounds was obtained with ultrasound technology and the application of suitable optimization modelling was essential to identify the optimized extraction conditions [17][18][19]. ...
... This behavior was similarly reported in a recent study dealing with ultrasound extractions from carob pods, in which solvent concentration and solid to solvent ratio were among the three most dominant factors that influenced the polyphenols recovery, while, conversely to our finding, the other determinant factor was the sonication power [17]. Probably, this difference could be ascribed to the use by Christou et al. [17] of an ultrasonic probe system in their experiment; indeed, a previous research have demonstrated that, when an ultrasonic water bath is employed for extracting D-pinitol from carob pods, the sonication power is not statistically significant [19]. As regards the other factors tested in our study, negligible importance of extraction temperature and time was particularly unexpected. ...
Article
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Carob pulp has recently received great attention due to its considerable content of polyphenols having a wide range of health promoting effects. In this work, ultrasound assisted extraction was optimized sequentially using a screening Plackett–Burman design and non-standard central composite design coupled to response surface methodology and desirability function statistical tools, to find the best conditions for the extraction of nine polyphenols from carob pods. The gathered mathematical models showed that the highest significant factors influencing the extraction of all compounds were solid–solvent ratio, solvent concentration, and particle size, with the optimal results obtained at values of 0.2 g/mL, 40% ethanol, and 0.3 mm, respectively. Extraction temperature, time, sonication power, and frequency were set at 35 °C, 15 min, 100 W, and 37 kHz, respectively. These parameters help to reduce energy costs and to obtain the best possible extraction of polyphenols.
... Myo-inositol is a sugar polyalcohol which participates in plant development by promoting the biosynthesis of molecules responsible for the cell wall structure [33]. Our results are in agreement with previous results, where cyclitols (myo-inositol, d-pinitol, etc.) were mostly extracted at higher UAE solvent volumes and extraction times [34] (Tables S2a and S5) (Groups 2,3 in yellow). As stated Extracts with low carotenoid yields (Group 1, green dots) were enriched in branched-chained hydrophobic amino acids (valine, leucine, and isoleucine) (Figure 8b). ...
... Myo-inositol is a sugar polyalcohol which participates in plant development by promoting the biosynthesis of molecules responsible for the cell wall structure [33]. Our results are in agreement with previous results, where cyclitols (myo-inositol, d-pinitol, etc.) were mostly extracted at higher UAE solvent volumes and extraction times [34] (Tables S2a and S5) (Groups 2,3 in yellow). As stated in other studies [35], MAE extracts containing inositol were obtained at short extraction times (≤20 min) and high solvent/material ratios, which is a finding that is in accordance with our study (Tables S2b and S5) (Groups 2,3 in yellow). ...
Article
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Traditional extraction remains the method-of-choice for phytochemical analyses. However, the absence of an integrated analytical platform, focusing on customized, validated extraction steps, generates tendentious and non-reproducible data regarding the phytochemical profile. Such a platform would also support the exploration and exploitation of plant byproducts, which are a valuable source of bioactive metabolites. This study deals with the incorporation of (a) the currently sub-exploited high energy extraction methods (ultrasound (UAE)- and microwave-assisted extraction (MAE)), (b) experimental design (DOE), and (c) metabolomics, in an integrated analytical platform for the extensive study of plant metabolomics and phytochemical profiling. The recovery of carotenoids from apricot by-products (pulp) is examined as a case study. MAE, using ethanol as solvent, achieved higher carotenoid yields compared to UAE, where 1:1 chloroform-methanol was employed, and classic extraction. Nuclear magnetic resonance (NMR)-based metabolomic profiling classified extracts according to the variations in co-extractives in relation to the extraction conditions. Extracts with a lower carotenoid content contained branched-chain amino acids as co-extractives. Medium carotenoid content extracts contained choline, unsaturated fatty acids, and sugar alcohols, while the highest carotenoid extracts were also rich in sugars. Overall, the proposed pipeline can provide different the phytochemical fractions of bioactive compounds according to the needs of different industrial sectors (cosmetics, nutraceuticals, etc.).
... In recent years, cyclitols in general, and D-pinitol in particular, have been receiving increasing attention because of its occurrence in foods and medicinal plants, including soybean (Glycine max), carob pod (Ceratonia siliqua), ice plant (Mesembryanthemum crystallinum), fenugreek seed (Trigonella foenumgraecum), and some species of Retama genus (Lee et al. 2014;Tetik and Yüksel 2014;González-Mauraza et al. 2016;Lahuta et al. 2018;Zhang et al. 2019;Christou et al. 2019). Moreover, D-pinitol has been suggested to possess multifunctional properties including antidiabetic (Gao et al. 2015), antioxidant (Lee et al. 2019), cancer chemopreventive (Rengarajan et al. 2012), anti-inflammatory (Zheng et al. 2017) and antitumoral (Lin et al. 2013) among others. ...
... Negishi et al. 2015;Zhang et al. 2019). The main industrial source to obtain D-pinitol is through the extraction from carob pod and soybean leaves (López-Sánchez et al. 2018) by ultrasoundassisted extraction (Tetik and Yüksel 2014). ...
Article
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d-Pinitol (3-O-methyl-d-chiro-inositol) is a cyclitol nearly ubiquitous in the Leguminosae and Pinaceae families. It plays an important role in plants as physiological cellular modulator and chemical defense against unfavorable environmental conditions, such as water deficit and high level of salinity. Plants rich in d-pinitol are being used in traditional medicine as empirical treatment for diabetes, inflammation, cancer or infections. This review summarizes the extensive literature published about d-pinitol biosynthesis, plant distribution, biological activities and pharmacological studies, including in vitro, in vivo, and clinical trials.
... Ceratonia siliqua L. (C. siliqua L.) or carob, belongs to the family of Leguminosae [35] and the subfamily of Caesalpinaceae [36]. It is widespread in the Mediterranean basin [37]. ...
... It is widespread in the Mediterranean basin [37]. Carob is a perennial tree, evergreen [36], dioecious with some hermaphrodite forms [27]. C. siliqua L., naturally grown in arid regions [38], and is a salinity and drought-resistant plant [27,35]. ...
Article
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Ceratonia siliqua L. is a Mediterranean medicinal plant traditionally cultivated for its ethnopharmacological benefits, such as antidiarrheal, antidiabetic, enhance acetylcholine, antioxidant, antiatherosclerotic, and for its possible anti-neurodegenerative potential. The aim of the present study was to evaluate the chemical composition, as well as the cognitive-enhancing, anxiolytic, and antioxidant activities of the aqueous extract from C. siliqua (CsAE) leaves against 6-hydroxydopamine (6-OHDA) zebrafish Parkinson’s disease (PD) model. CsAE (0.1, 0.3, and 1 mg/L) was administered by immersion to zebrafish (Danio rerio) for eight consecutive days and one hour before each behavioral test of each day, while 6-OHDA (250 µM) treatment was supplied one day before the novel tank diving test (NTT). Qualitative and quantitative analyses were performed by the ultra-high-performance liquid chromatography (UHPLC) analysis. The memory performance was evaluated through the NTT and Y-maze tests. Additionally, the in vitro and in vivo antioxidant status and acetylcholinesterase (AChE) activity was also assessed. Our finds demonstrated that CsAE presented positive antioxidant and anti-AChE activities, which contributed to the improvement of cognitive function in the 6-OHDA zebrafish PD model.
... Indeed, they have always been popular for human consumption because of their high sugar content [9] and perceived beneficial effects for health [10]. Fruits are used for beverage and syrup preparation [5,11], while both the pulp and seeds are used for animal feed and industrially exploited to extract valuable products [12]. Particularly, locust bean gum (LBG), marketed as E410 [6,13], has food and non-food uses [14]. ...
... Particularly, locust bean gum (LBG), marketed as E410 [6,13], has food and non-food uses [14]. The pulp has been evaluated as a cacao substitute [12] and use for the industrial production of crystallized sucrose [14] and even as a substrate for bioethanol and citric acid production [11,15]. The fruits are used in traditional and modern medicine for the prevention and treatment of several diseases [16] due to their biological activities, including antioxidant, antidiarrheal, antimicrobial [17] and antiproliferative activities, among others [15]. ...
Article
Carob leaves, the main residues of the carob tree, were investigated as a renewable and abundant source of bioactive compounds for fish aquaculture. Aqueous and ethanolic extracts obtained from carob leaves were characterized in terms of biochemical composition, antiradical and cytotoxic effects and immunostimulant and antibacterial activities. The ethanolic extract showed higher levels of total phenolics, flavonoids and condensed tannins and higher antioxidant activity than the aqueous extract. No significant immunostimulant effects were observed on gilthead seabream (Sparus aurata) head kidney leucocytes (viability, phagocytosis and respiratory burst activities and peroxidase content) after incubation for 24 h with different extracts. Furthermore, the ethanolic extracts used at 0.5, 0.75 and 1 mg mL-1 and aqueous extracts at 1 gmL-1 had a cytotoxic effect on PLHC-1 cells. When the bactericidal activity was tested against three fish pathogenic bacteria (Vibrio harveyi, Vibrio anguillarum and Photobacterium damselae) notable activity of the different extracts was detected against P. damselae at all three concentrations. A similar effect was demonstrated against V. haryeri when ethanolic extracts were used in the same range of concentrations. This work demonstrates interesting in vitro effects of carob leaf extracts and suggests it could be used as an alternative to chemical compounds with farmed fish. The concentration and nature of the extracts were very important in terms of any positive results.
... For the carob fruit, the conditions of the ultrasound-assisted extraction method are stated as 40 kHz frequency, 45-297 W power, at 30 to 50 ºC, 30 to 120 minutes. N. Tetik and E. Yuksel [12] studied on the optimization of extraction conditions of D-pinitol compound by using carob ultrasound and four independent variables. It was stated that these variables are temperature, ultrasonic power, dilution rate and time. ...
... They suggest that their approach allows a potential energy savings as much as 48% according to conventional approaches. There are more studies about the extractions, Taguchi methods, and the heat and mass transfers in the literature [12], [15]-[18]. ...
Article
The carob, a perennial plant, is grown in regions where the Mediterranean climate is dominant. Because of its properties, it is preferred in many sectors especially in the food and health sectors. Carob is mostly used as sugar and molasses. Moreover, seeds of carob are also used as thickening material in the food sector and its residue is utilized as animal feeding stuff as well. Molasses are mostly produced from carob, grape, mulberry, apple, and pear for many years in Turkey. Molasses production is different from each other with regard to the structure of each fruit. Molasses are produced by pressing in the event of soft. The molasses of hard dried fruits such as carobs which cannot be pressed are obtained by extraction method using water. The parameters which are important for the quality of product such as extraction temperature and duration are not taken into account in the carob molasses obtained by traditional methods. Increasing the amount of water in extraction decreases production efficiency and quality while increasing energy consumption. In this study, the effects of parameters such as water quantity, extraction temperature, duration and the batch number that affect the quality of molasses were experimentally investigated by being used Taguchi method.
... Žlabur et al. [55] investigated the influence of conventional and ultrasound-assisted extraction (frequency, time, and temperature) on the content of bioactive compounds including flavonoids obtained from lemon balm and peppermint leaves [55]. Meanwhile, Tetik and Yüksel [56] used UAE for extraction of d-pinitol from Isolation, Separation, and Preconcentration of Biologically Active Compounds from Plant… carob bods and studied the influence of different parameters such as temperature, ultrasonic power, dilution rate (material:water ratio), and time. Those authors reported that the highest concentration of d-pinitol was 11.98 g L −1 , obtained using temperature of 50 °C, ultrasonic power of 207 W, dilution rate of 1:4, and extraction time of 120 min [56]. ...
... Meanwhile, Tetik and Yüksel [56] used UAE for extraction of d-pinitol from Isolation, Separation, and Preconcentration of Biologically Active Compounds from Plant… carob bods and studied the influence of different parameters such as temperature, ultrasonic power, dilution rate (material:water ratio), and time. Those authors reported that the highest concentration of d-pinitol was 11.98 g L −1 , obtained using temperature of 50 °C, ultrasonic power of 207 W, dilution rate of 1:4, and extraction time of 120 min [56]. ...
Article
Full-text available
Development of efficient methods for isolation and separation of biologically active compounds remains an important challenge for researchers. Designing systems such as organomineral composite materials that allow extraction of a wide range of biologically active compounds, acting as broad-utility solid-phase extraction agents, remains an important and necessary task. Selective sorbents can be easily used for highly selective and reliable extraction of specific components present in complex matrices. Herein, state-of-the-art approaches for selective isolation, preconcentration, and separation of biologically active compounds from a range of matrices are discussed. Primary focus is given to novel extraction methods for some biologically active compounds including cyclic polyols, flavonoids, and oligosaccharides from plants. In addition, application of silica-, carbon-, and polymer-based solid-phase extraction adsorbents and membrane extraction for selective separation of these compounds is discussed. Potential separation process interactions are recommended; their understanding is of utmost importance for the creation of optimal conditions to extract biologically active compounds including those with estrogenic properties.
... The availability of D-pinitol in Locust Bean Gum may be responsible for the anti-diabetic benefits since it controls blood sugar levels in Type II diabetes mellitus patients by enhancing insulin sensitivity (Tetik and Yüksel 2014). Bates et al (2000) shows that the percentage of blood sugar absorption in the D-pinitol sample was approximately equivalent to the percentage of insulin infusion activity, indicating that D-pinitol displays an insulin-like actions. ...
Article
The Locust Bean (Ceratonia siliqua L.) is an ancient Mediterranean fruit that is used to make locust bean gum from seeds, which is a popular ingredient in many foods today. Locust Bean fruit and Gum are rich in bioactive compounds that can be helpful in the treatment of conditions involving the digestive system, as well as cancer, hyperlipidemia, and diabetes. The locust bean gum is a polysaccharide extracted from the endosperm of the locust bean seed through different thermomechanical or chemical processes. It is an approved food additive with the European number E410 and a number of different food uses. It is a galactomannan and it is frequently used in dairy products for its water-binding and thickening properties to improve their rheological properties. This review aims to study the functional, and nutritional characteristics of Locust Bean Gum, the extraction of Locust Bean Gum, as well as its applications in the food sector and its impacts on dairy product processing.
... Ten grams of it is adequate to decrease the sugar level in type II diabetes as compared to the normal dose (10 mg D-pinitol/kg body weight). Tetik and Yüksel (2014) proposed that D-pinitol could have strong measures with insulin, and therefore improve glycemic control by evaluating its effectiveness in diabetes animal models. The study also reported that D-pinitol induced increased glucose absorption in the L6 line of muscles, indicating its presence in the glucose metabolic pathway of muscles rather than the increased development or action of insulin (Ali, Ain, et al., 2021;Coviello et al., 2015). ...
... The extraction efficiency of plant active ingredients is greatly influenced by several factors including their storage conditions, chemical nature, especially extraction conditions as well as the use of extraction methods [11]. In many previous studies, the traditional extraction methods such as solvent extraction (decoction, digestion, maceration, hot continuous extraction), distillation, cold compression, countercurrent extraction, as well as various newer extraction techniques including pressurized liquid extraction, supercritical fluid extraction, microwaves assisted extraction and ultrasound assisted extraction were successfully applied to extract the vegetal compounds [12][13][14][15][16][17]. Compared with the traditional extraction methods, extraction assisted by ultrasound has exhibited many advantages such as less amount of solvent, shorter extraction time and lower operating temperature with higher extraction rate. ...
Article
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In this work, multi-frequency ultrasound (working modes for the single-, dual- and tri-frequency in simultaneous ways) was applied to extract bioactive compounds from purple eggplant peels. The single-factor experiments were performed by varying six independent variables. A six-level-five-factor uniform design (UD) was further employed to evaluate the interaction effects between different factors. It was found that extraction temperature and extraction time significantly affected the total phenolic content (TPC), whereas the total monomeric anthocyanins (TMA) was mainly influenced by ethanol concentration, extraction temperature and solid-liquid ratio. Based on partial least-squares (PLS) regression analysis, the optimal conditions for TPC extraction were: 53.6 % ethanol concentration, 0.336 mm particle size, 44.5 °C extraction temperature, 35.2 min extraction time, 1:43 g/mL solid-liquid ratio, and similar optimal conditions were also obtained for TMA. Furthermore, the TPC and TMA extraction were investigated by ultrasound in different frequencies and power levels. Compared with single-frequency (40 kHz) and dual-frequency ultrasound (25 + 40 kHz), the extraction yield of TPC and TMA with tri-frequency ultrasound (25 + 40 + 70 kHz) increased by 23.65 % and 18.76 % respectively, which suggested the use of multi-frequency ultrasound, especially tri-frequency ultrasound, is an efficient strategy to improve the TPC and TMA extracts in purple eggplant peels.
... The writers suggested the Ultrasonic assisted extraction as an alternative to conventional hot water extraction to recover D-pinitol from the carob pods. It is an advantageous alternative because it reduces the extraction time and thus the energy consumption 37 . ...
... Industrially, carob pulp is mainly used as syrups, cocoa substitutes (roasted powder), or antidiarrheal preparations (tannin-rich fractions). In traditional medicine, carob pulp is recommended for the treatment of GIT disorders as an antidiarrheal remedy [2], and as an antitussive agent [3]. Products of insoluble carob dietary fiber demonstrated cholesterol-lowering effects [4]. ...
... Compared to the maceration method, the highest yield obtained by UAE is justified by enhanced oil removal. The ultrasound process modifies the plant tissue structure through rupturing, increasing porosity and intercellular distances; thus, it decreases the resistance to mass transfer from the solute, which increases the penetration of solvent into the plant tissue (Tetik & Yüksel, 2014;Yingngam et al., 2014). Similar results have also been reported by other authors in the extraction of different plant species, in which UAE was more efficient than the conventional methods of maceration and Soxhlet extractions (Chen et al., 2014;Palsikowski et al., 2020;Santos et al., 2021;Stevanato & da Silva, 2019). ...
Article
In this study, clove leaves (Syzygium aromaticum) were subjected to ultrasound-assisted extraction (UAE) with ethanol as the solvent, following a central composite design to evaluate the effects of time, amplitude, solvent/sample ratio, and temperature on the yield, eugenol content, and antioxidant capacity of the extracts. The results were compared with those obtained using the conventional method of maceration (ME). The optimum conditions for extract yield were achieved with an extraction time of 25 min, amplitude of 85 %, solvent/sample ratio of 35 mL g⁻¹, and temperature of 70 °C, and the result (14.63 wt%) was three times higher than that of conventional extraction. Eugenol was detected in the extracts obtained by both methods, with the highest yield of 2.94 g eugenol kg leaves⁻¹ obtained in the UAE method, while the ME method achieved 1.36 g eugenol kg leaves⁻¹. In general, the extracts exhibited high antioxidant capacities.
... This natural compound, related to the important family of inositols, is present in carob in high levels and increases this Leguminosae's value due to its pharmacological importance related to anti-cancer, anti-diabetic, antioxidant, and anti-ageing properties . Besides the classic extraction associated with the syrup carob production, D-pinitol extraction from carob pulp was studied using microwave (Ersan et al., 2020), supercritical CO 2 (Cháfer & Berna, 2014) and ultrasound (Tetik & Yüksel, 2014) techniques. Finally, the carob seed consists of three parts: the peel (husk), the endosperm and the germ. ...
Article
Background Carob (Ceratonia siliqua L.) is an evergreen tree that belongs to the Leguminosae family and is typical of the Mediterranean basin. It is well known for its valuable locust bean gum obtained from carob seeds. However, the food industry can obtain different carob products from carob fruit after processing. Carob products are good sources of dietary fibre, sugars, and a range of bioactive compounds such as polyphenols and D-pinitol. Scope and approach Bioactive compounds present in carob fruit and its derived products help control many health problems such as diabetes, heart diseases, and gastrointestinal disorders due to their anti-hyperglycaemic, antioxidant, and anti-inflammatory activities. So, carob products have a great potential to be used as a functional food ingredient. Key findings and conclusions This article focuses on carob characteristics and processing, chemical composition, health benefits, and applications in food formulations to explore the potential of carob in developing a wide variety of health-beneficial food products.
... Ultrasound-assisted extraction (UAE) is a modern extraction technique suitable for cyclitols' extraction, with some advantages (solvent amount reduction, low energy consumption, and time-saving) compared to classical methods. The principle of UAE is the utilization of ultrasound in order to create cavitation bubbles inside the liquid solvent meant to induce disruption of the plant cell wall and speed up the solvent penetration in plant material (Tetik and Yüksel 2014). ...
Chapter
In food and biological systems, the main function of tocochromanols is antioxidant action – they deactivate free radicals and protect lipids from peroxidation (autoxidation). In addition to the antioxidant role of vitamin E and protection against oxidative stress, the “non-antioxidant” functions of vitamin E, including cell signaling and antiproliferation, is also described. Tocopherols and tocotrienols are not the only compounds classified as tocol derivatives. This chapter also includes an overview of the properties and occurrence of other forms of tocols (including: tocomonoenols, tocodienols, and plastochromanol-8). Content of tocochromanols in food may be determined using a wide range of analytical techniques. Capillary gas chromatography and high performance liquid chromatography coupled with various detection systems and mass spectrometers enable identification of individual compounds. In the analysis of these compounds, spectroscopic methods are also being developed. The principles of these techniques are discussed in the chapter and examples of their applications are also provided.
... According to 2018 data from the Food and Agricultural Organization of the United Nations, its production quantity and yield were used to produce several products such as locust bean gum, sweets, biscuits, and traditional carob concentration Yatmaz and Turhan, 2018). On the other hand, the carob is rich-sugar and therefore can be used for the production of many value-added products such as citric acid (Lingappa et al., 2007), lactic acid (Germec et al., 2018a;Turhan et al., 2010a), mannitol (Carvalheiro et al., 2011), biocontrol agent (fungicide: Pantoea agglomerans PBC-1) (Manso et al., 2010), ethanol (Ercan et al., 2013;Germec, 2014;Germec et al., 2019a;Germec et al., 2018bGermec et al., 2016;Germec et al., 2015Germec et al., , 2019cTurhan et al., 2010b), D-pinitol (Oziyci et al., 2015;Tetik et al., 2011;Tetik and Yüksel, 2014), β-mannanase Germec et al., 2017;Karahalil et al., 2019a;Karahalil et al., 2019b;Yatmaz et al., 2016a;Yatmaz et al., 2016b), and inulinase Ilgın et al., 2019). Accordingly, as a continuation of our previous study (Ilgın et al., 2019), carob has been used as a carbon source in the production of Aspergillus niger A42 inulinase in the submerged fermentation in this study, due to its high level of sugar content (62-67% total soluble solids, 34-42% sucrose, 7-10% glucose, and 10-12% fructose) (Yatmaz and Turhan, 2018). ...
Article
This study aimed to optimize inulinase production conditions from carob extract by using the Box-Behnken Design of Response Surface Methodology, to purify partially with ultrafiltration, and to model kinetically the inulinase fermentation. Based on the results, the optimal conditions were 250 rpm agitation speed, 2.3% inoculum size (v/v), and 135 mL medium volume, which yielded 1560.17 U/mL inulinase activity, 1198.36 U/mL invertase-type activity, 1.30 I/S ratio, 163.06 U/mL/d maximum inulinase fabrication rate, and 193.37 U/mL/d maximum invertase-type fabrication rate. With the ultrafiltration process, the inulinase and invertase-type activities were increased to 6278.69 and 7622.39 U/mL with 1.19 and 1.50 purification coefficients, respectively. Regarding modeling with the Luedeking-Piret model, enzyme and protein productions were not related to the substrate depletion due to negative a values. Consequently, carob extract can be evaluated for the fabrication conditions of A. niger inulinase and the purified enzyme can be used for the fabrication of fructooligosaccharides.
... The polyphenols were the most important secondary metabolites and considered as an interesting compound define the nutritional and functional fruits quality (12,38). As the primary metabolites, this groups of molecules recorded important variation during ripening (12), since some authors revealed that during ripening of fruits the evolutionary behavior of secondary metabolisms was highly associated with that of primary ones (28,39). ...
Article
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The Ceratonia siliqua fruits contain several substances known to have high adaptability to environmental conditions. The aim of this paper is to evaluate the changes in physicochemical properties of different Tunisian provenances of carob pulps harvested at three ripening stages. Furthermore, six provenances were investigated during the ripening process in terms of their moisture, ash, minerals, bioactive compounds, antiradical activity and sugar profile. The results demonstrated that all examined parameters are highly influenced by geographic origin. Concerning ripening impact, our data showed that water and ash content significantly decreased during the development of six provenances, as well as the bioactive and mineral contents. Thus, the total polyphenols (TP), total flavonoids (TF) and condensed tannins (CT) contents exhibited the highest levels in the unripe fruits. The antiradical activity trend was positively correlated to the behavior of the bioactive compounds content. Moreover, the sucrose, glucose and fructose were the main sugar qualified and quantified in carob pods at different ripening stages. At the maturity stage, the monosaccharide contents (glucose and fructose) were slightly reduced, while, the sucrose was rapidly accumulated. In conclusion, the ripening process diversely affected the nutritional composition and generally extended the exploitation of carob fruits. The study could provide valuable information about the suitability of carob pods at different maturity stages as potential biomaterials for nutraceutical applications.
... The writers suggested the Ultrasonic assisted extraction as an alternative to conventional hot water extraction to recover D-pinitol from the carob pods. It is an advantageous alternative because it reduces the extraction time and thus the energy consumption 37 . ...
Chapter
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The carob is a dome-shaped evergreen tree that is a member of the pea family (Fabaceae). Its fruit has been used for human consumption and as animal feed in the Mediterranean countries for centuries and was also widely used as a herbal remedy in traditional folk’s medicine. In this paper, an in-depth literature review was conducted about this species discussing its history, origins, main current uses, components (both nutrient and bioactive), biological activities, and potential applications as the source of sustainable ingredients and products. Among the many bioactive compounds that were found in carob, the most well studied are polyphenols. The levels of these compounds were found to vary depending on many factors, such as the variety, plant part, geographic location, roasting and extraction conditions, and even analysis methods. In the light of these researches, it was recognized that carob offers several biological activities including antioxidant, anticancer, and anti-diabetic due to the presence of a high quantity of pinitol and antibacterial. Rich in sugars, proteins, and minerals, the carob has a vast range of industrial applications such as cacao substitute, sugars substitute, free from gluten making it cereal-derived foods for celiac people.
... Furthermore, spectroscopic techniques like nuclear magnetic resonance (NMR) and infrared spectroscopy (IR) were also employed [5]. The ultrasound-assisted extraction (UAE) of D-pinitol from carob pods using response surface methodology (RSM) by optimization of the affected parameters (temperature, ultrasonic power, dilution rate and time) was also reported [10]. Additionally, D-pinitol was isolated from carob pods using supercritical fluid extraction (SFE). ...
Article
D-pinitol (3-O-methyl-D-chiro-inositol) is a well-known bioactive compound with anti-diabetic and anti-oxidant biological functions. A gas chromatography–mass spectrometry (GC–MS) method was developed for its quantitation in carob syrup, flesh and seed samples originated from Cyprus. The analysis was performed after derivatization of carbohydrates and polyols into trimethylsilyl ether derivatives. D-pinitol was determined in 13 carob syrup samples, in concentrations ranging 65.71 ± 4.60 – 77.72 ± 5.44 mg/g (mean: 68.58 ± 4.80 mg/g, n = 13). In two commercial samples, it was determined in relative medium-low concentrations (21.96 ± 1.54 and 44.71 ± 3.13 mg/g), revealing possible adulteration; however, this needs further investigation. Similarly, it was determined in high concentrations in carob flesh samples, in concentrations ranging 53.20 ± 3.72 – 54.58 ± 3.82 mg/g (mean: 53.81 ± 3.76 mg/g, n = 3). On the other hand, seed samples proved very poor in D-pinitol (<LOD). Therefore, bioprospecting of carob fruit and syrup is highlighted. Compared to other plants or legumes, carob appears to be the richest source of D-pinitol, highlighting carobs role as a functional organic food. The historical and cultural association of Cyprus with carobs is linked with traditional foods and habits.
... [2,7,8] The main polyphenolic constituents isolated from carob pods are reported to be insoluble, highly polymerised condensed tannins containing a flavan nucleus. [9] Other research has analysed the cyclitol content of the pods by high-performance liquid chromatography (HPLC), [10][11][12] seed germ amino acid content via HPLC, and the presence of fatty acids employing gas chromatography (GC). [13] Recently, analysis of carob flesh and pods was conducted using FTIR spectroscopy and this technique was used to assess the origin and type of carob material. ...
Article
Studies of the phytochemistry of carob (Ceratonia siliqua) leaf material are extremely limited. This report features the second natural product isolation study of carob leaves and the first such investigation of C. siliqua grown in Australia. Investigation of leaf material from seven carob cultivars using pressurised hot water extraction (PHWE) revealed the presence of high levels of myricitrin, d-pinitol, and sucrose in addition to the previously unreported natural product siliquapyranone {(2R,3R,4S,5R,6R)-5-hydroxy-6-(hydroxymethyl)-2-(((2S,4S)-2-methyl-6-oxotetrahydro-2H-pyran-4-yl)oxy)tetrahydro-2H-pyran-3,4-diyl bis(3,4,5-trihydroxybenzoate)}. Siliquapyranone represents a biosynthetic fusion of conventional 2,3-gallate esters on a β-glucose tannin with a hydroxytetrahydro-2H-pyran-2-one-related non-tannin tetrahydropyran-2-one, parasorboside. Preliminary biological testing indicates that siliquapyranone exhibits weak activity against both tumour and normal cell lines. This suggests that, like most tannins and parasorboside, siliquapyranone may act as an antifeedant.
... And it can fit out a multivariate equation to optimize the parameters after setting up a proper experimental design [19,20]. A large quantity of previous literatures has explained the methodology is efficient and reasonable [21][22][23]. The objectives of this report were to investigate the effect of ultrasound on the extraction efficiency of RBP, and optimize the parameters of extraction conditions using RSM. ...
Article
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This report used Response Surface Methodology (RSM) to analyze the conditions that extracting polysaccharide compound from Radix Bupleuri using ultrasonic wave. For determining the optimal extraction conditions, four independent variables, temperature (℃), ultrasonic intensity (UI, W/cm²), dilution rate (water-material ratio, mL/g) and time (min), were investigated using Box-Behnken design. In the results, the best condition after optimization was dilution rate of 35.0:1, UI of 24.5 W/cm², temperature of 69.5℃ and time of 14.6 min. Extraction efficiency was 7.67% and the purity reached 44.14%. It illustrates that the ultrasound-assisted extraction (UAE) was efficient and suitable for extracting polysaccharide from Radix Bupleuri. This paper also investigated the antioxidant activity of Radix Bupleuri polysaccharide (RBP) on superoxide anion radical, hydroxyl radical, and 2,2-diphenyl-1-picry-hydrazyl (DPPH), in vitro experiment. The result indicated that RBP could remarkably sweep away the hydroxyl radical, and had the capacity for clearing away superoxide radical and DPPH.
... For the purposes of the technological innovation processes and rural development strategies envisaged in the Community programs, it is therefore necessary to look at the possible alternatives and, among them, the second generation biofuels from biomass production, which, as was pointed out in this work, could be an interesting opportunity in the process of realization of agricultural integrated and multi-functional company, also for typical rural areas ). The opportunities offered by the rural development policy provide for the possibility of financing investments at or near farms, for example to process biomass and to mobilise biomass unused by farmers (Tetik and Yüksel, 2014). Therefore, in a national scene which sees the agricultural sector that, even if it represents the primary foundation of the national and regional economy, highlights more and more limits of survival and structural difficulties, a particular attention to the regional peculiarities seems today imperative. ...
Article
The present work intends to evaluate the possibility to produce bioethanol through fermentation of the carob. This sustainable process could revive the economy of rural areas of the Mediterranean basin. In particular in Italy, where you can find the largest cultivation of carob in the world. Italy is the leading producer of carob in the world and yet it is difficult to find this fruit and its derivatives such as syrups and flour on sale. The feasibility study has sought to evaluate the convenience of producing energy from the carob tree. They wanted to show how the exploitation of energy from biomass residual can make it possible to transform the waste materials in energy products that permit the production of renewable energy from biomass without the use of agricultural land for energy purposes. © 2018, SRAC - Romanian Society for Quality. All rights reserved.
... Recently, ultrasonic-assisted extraction (UAE) has been developed for the extraction of bioactive compounds from natural sources (Bimakr et al., 2012). Its advantages including acceleration of extraction speed, improvement of the extraction efficiency and economization of energy consumption have been well demonstrated (Ahmad, Alkharfy, Wani, & Raish, 2014;Chen et al., 2010;Esclapez, García-P erez, Mulet, & C arcel, 2011;Li, Sun, Xu, & Sun, 2012;Tetik & Y€ uksel, 2014). ...
Article
An ultrasound‐assisted procedure for the extraction of water‐soluble polysaccharides from Enteromorpha tubulosa was studied by using response surface methodology. Three independent variables including extraction time, extraction temperature, and ratio of liquid to raw material were investigated by single‐factor experiments. A three‐factor‐three‐level Box–Behnken design was adopted to optimize the extraction process parameters. A highly significant second‐order polynomial equation was fitted by using multiple regression analysis. The optimal extraction conditions were obtained as follows: extraction time 36 min; extraction temperature 69 °C; and ratio of liquid to raw material 45 mL/g. By experiments with these conditions, the extraction yield was 16.04%, which was well matched with the predicted value. The obtained polysaccharides were evaluated for cytotoxicity in vitro against human breast cancer cell line MCF‐7 and the results showed that the polysaccharides possessed potent cytotoxicity. Practical applications Seaweeds are one of the largest numbers and species of marine plants, and their bioactive compounds, especially algal polysaccharides, have become the focus of research in the field of food and medicine. Moreover, many algal polysaccharides have been gradually applied to food and medicine owing to their varied biological activities, such as antivirus, antitumor, antiradiation, antimutation, antioxidation, and enhancing immunity. However, there is no universal extraction process for polysaccharides from the different seaweeds because of the different structures of the seaweeds and the varying compositions of algal polysaccharides. In the current research, an ultrasound‐assisted procedure for the extraction of water‐soluble polysaccharides from Enteromorpha tubulosa was studied by using response surface methodology, and the optimal extraction conditions were obtained so as to provide references for the mass productions in the factories.
... Both techniques GC-MS and GC-FID have been used for the analysis of different cyclitols present in sea buckthorn berries (Hippophaë rhamnoides) [14]. Other chromatographic techniques such as TLC [15], HPLC with different detectors like refractive index detector (RI) [16], evaporative light scattering detector (ELSD) [14], and MS [17] have also been applied for the determination, identification, and quantification of cyclitols and other phytochemicals [18,19]. In this study, Soxhlet extraction and SPE were involved as extraction and purification methods. ...
Article
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Plant research interest has increased all over the world, and a large body of evidence has been collected to show the huge potential of medicinal plants in various disease treatments. Medicago sativa L., known as alfalfa, is a rich source of biologically active components and secondary metabolites and was frequently used from the ancient times both as fodder crop and as a traditional medicine in the treatment of various diseases. Cyclitols, naturally occurring in this plant, have a particular interest for us due to their significant anti-diabetic, antioxidant, anti-inflammatory and anti-cancer properties. In the present study we revealed the isolation, the identification and the quantification of some cyclitols and sugars extracted from different morphological parts of alfalfa plant. Soxhlet extraction and solid phase extraction were used as extraction and purification methods, while for the analyses derivatization followed by gas chromatography with mass spectrometry was involved. The obtained results showed significant differences in the quantities of cyclitols and sugars found in the investigated morphological parts, ranging between 0.02 and 13.86 mg/g of plant in case of cyclitols, and in the range of 0.09 and 40.09 mg/g of plant for sugars. However, roots have the richest part of cyclitols and sugars in contrast to the leaves.
... Carob powder contains daily nutritional amount of potassium, calcium, magnesium, and iron [15,36]. It is reported that carob comprises a high amount of pinitol, which has beneficial effects on human health, such as the regulation of blood glucose levels and reduction of hyperlipidemia and inflammation [37,38]. Containing a large amount of bioactive compounds, carob kibble has shown good antioxidant activities [2,10,39,40], anticancer and antiproliferation effects [41], antidiabetic effect [42,43], cholesterol lowering effect [44,45], and antimicrobial effects [23] and it has positive effects on cardiovascular diseases [42,46]. ...
Article
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The main objective of this research was to compare physicochemical parameters, antioxidant activity, lipid composition, and sensory analysis of initial and roasted carob pod powder ( Ceratonia siliqua L.) obtained at different roasting temperatures. The roasted products became darker and the average moisture content, water activity, oil content, and sweetness values decreased at higher temperatures. Total polyphenol content and antioxidant activity increased with increasing roasted temperature. Oleic acid, linoleic acid, and palmitic acid were the main fatty acids present in carob oil. Results showed that the roasted carob pod powders are sweeter, have more caramel-like taste, and have more cacao-like aroma at lower roasting temperatures but have more astringent taste, coffee-like aroma, and roasted aroma at higher roasting temperatures.
... The seeds are used to produce locust bean gum; mainly used in the food industry (4). The pod of carob is rich in sugars (40-60 %, mostly sucrose), D-pinitol, minerals, dietary fibre and polyphenols (1,(5)(6)(7)(8)(9)(10). Pods are utilized as a processed carob syrup (pekmez in Turkish), carob powder for human consumption (1,11,12) as well as animal feed. ...
... The presence of D-pinitol in carob products could be responsible for the anti-diabetic effects as it regulates blood sugar level in patients with Type II diabetes mellitus by increasing insulin sensitivity [71]. Carob syrup is considered as a rich source of D-pinitol; as 10 g of it are sufficient, in comparison with the standard dose (10 mg D-pinitol/kg body weight), to lower the blood sugar level in type II diabetes [33]. ...
Article
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The contribution of natural products to the drug-discovery pipeline has been remarkable since they have served as a rich source for drug development and discovery. Natural products have adapted, during the course of evolution, optimum chemical scaffolds against a wide variety of diseases, including cancer and diabetes. Advances in high-throughput screening assays, assisted by the continuous development on the instrumentation’s capabilities and omics, have resulted in charting a large chemical and biological space of drug-like compounds, originating from natural sources. Herein, we attempt to integrate the information on the chemical composition and the associated biological impact of carob fruit in regards to human health. The beneficial and health-promoting effects of carob along with the clinical trials and the drug formulations derived from carob’s natural components are presented in this review.
... Sonication can be used to generate very fine emulsions from immiscible liquids, which produce the very large interfacial contact areas between the liquids and increase the mass transfer between two phases. This phenomenon leads to an upgrade in the extraction efficiency in a minimum time [28][29][30][31]. In these methods, the extractant is dispersed into the aqueous solution with the aid of ultrasound radiation. ...
... To establish these models, there is a need for process analysis to identify the main variables or parameters which are of relevance when running the process. Frequently, surface response methodologies are considered due to their simplicity (Tetik and Yüksel, 2014;Turhan, 2011), although many times the complexity of the process does not allow a general approach in changing situations (Bon et al., 2005). The best way to address this aspect is by mechanistic modeling, avoiding purely empirical approaches (Rodriguez et al., 2014). ...
... Ultrasound-assisted extraction is a novel method to effectively extract targeted components from plant products which has been proven to significantly increased extraction yield together with shorter time, lower temperature and smaller solvent [6]. Recently, many studies have reported that higher extraction yields could be achieved when an UAE method was adopted on many plant products, such as rutin from flower buds of Sophora japonica [7], oil from tobacco (Nicotiana tabacum L.) seeds [8], carvone and limonene from caraway seeds [9], polyphenols from black tea [10], extraction of carotenoids [11], pectins from grape pomace [12], D-pinitol from carob pods [13], and vanillin from vanilla pods [14]. Those studies mainly looked at optimization of other extraction conditions with regards to efficiency and/or yield. ...
Article
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A new method has been proposed for enhancing extraction yield of rutin from Sophora japonica, in which a novel ultrasonic extraction system has been developed to perform the determination of optimum ultrasonic frequency by a two-step procedure. This study has systematically investigated the influence of a continuous frequency range of 20-92kHz on rutin yields. The effects of different operating conditions on rutin yields have also been studied in detail such as solvent concentration, solvent to solid ratio, ultrasound power, temperature and particle size. A higher extraction yield was obtained at the ultrasonic frequency of 60-62kHz which was little affected under other extraction conditions. Comparative studies between existing methods and the present method were done to verify the effectiveness of this method. Results indicated that the new extraction method gave a higher extraction yield compared with existing ultrasound-assisted extraction (UAE) and soxhlet extraction (SE). Thus, the potential use of this method may be promising for extraction of natural materials on an industrial scale in the future. Copyright © 2015 Elsevier B.V. All rights reserved.
... Therefore, UAE is a highly efficient method with reduced solvent-and time-consumption. Esclapez et al. (2011) reported that several process variables: ultrasonic power, frequency, extraction temperature, reactor characteristics and solvent-sample interaction can influence the extraction [22,23]. Mathematical modeling is an effective statistical model it include theoretical and statistical model for investigating the influences of different factors on extraction, as well as the search for the optimal conditions [24]. ...
Article
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This study reports on the optimization of the extraction conditions of cordycepin from Cordyceps militaris by using ultrasonication. For this purpose, the orthogonal experimental design was used to investigate the effects of factors on the ultrasonic-assisted extraction (UAE). Four factors: extraction time (min), ethanol concentration (%), extraction temperature (°C) and extraction frequency (kHz), were studied. The results showed that the highest cordycepin yield of 7.04 mg/g (86.98% ± 0.23%) was obtained with an extraction time of 60 min, ethanol concentration of 50%, extraction temperature of 65 °C and extraction frequency of 56 kHz. It was found that the cordycepin extraction yield increased with the effect of ultrasonication during the extraction process. Therefore, UAE can be used as an alternative to conventional immersion extraction with respect to the recovery of cordycepin from C. militaris, with the advantages of shorter extraction time and reduced solvent consumption.
... It was obvious that the UAE resulted in a higher efficiency concerning disruption of plant material compared to a conventional heat reflux extraction. This is attributed to the fact that ultrasonic cavitation creates shear forces to disrupt cell walls, followed by enabling solvent to penetrate into the plant tissue to dissolve phenolic compounds into the surrounding solvent [12] . Similar results were also reported for other plants [17] . ...
Article
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Objective: To optimize the processing parameters for phenolic compounds extracted from Cratoxylum formosum ssp. formosum leaves using an ultrasound-assisted extraction and to evaluate its protective ability against H2O2-induced cell death. Methods: The influence of three independent variables including ethanol concentration (%), extraction temperature (°C) and extraction time (min) on the extraction yield of phenolic compounds were optimized using a central composite design-based response surface methodology. The obtained extract was assessed for its antioxidant activity by DPPH(•) and ABTS(•)(+) methods. Cellular protective ability against H2O2-induced cell death was evaluated on HEK293 cells using the MTT assay. Results: The optimal conditions to achieve maximal yields of phenolic compounds were ethanol concentration of 50.33% (v/v), temperature of 65 °C, and extractiontion time of 15 min. The yield of phenolic compounds was (40.00±1.00) mg gallic acid equivalent/g dry powder which matched well with the values predicted from the proposed model. These conditions resulted in a higher efficiency concerning the extraction of phenolics compared to a conventional heat reflux extraction by providing shorter extraction time and reduced energy consumption. 5-O-caffeoylquinic acid identified by high performance liquid chromatography-diode array detector-electron spin ionization-mass spectrometry was the major compound in the obtained extract [(41.66±0.07) mg/g plant extract]. The obtained extract showed a strong ability to scavenge both DPPH(•) and ABTS(•)(+) free radicals and exhibited additionally good ability to protect HEK293 cells death against oxidative stress. Conclusions: These results indicate the suitability of ultrasound-assisted extraction for the extraction of phenolic compounds from Cratoxylum formosum ssp. formosum leaves. This phenolic-enriched extract can be used as valuable antioxidant source for health benefits.
... The importance of d-pinitol for human health and the increasing interest in drugs obtained from natural sources are an impetus for the extraction of this compound from vegetable raw materials. d-Pinitol can be found in several vegetable sources as carob pods, soybean leaves, Bougainvillea flowers, etc. [7] but its recovery, as well as the recovery of various other cyclitols from plants is generally accomplished by laborious separation processes [11]. For example, isolation of inositols and polyhydric alcohols has been attempted by partition chromatography with ion-exchange resins and by thin-layer chromatography [12][13][14][15][16]. ...
Article
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Carob is botanically called as Ceratonia siliqua and belongs to the Legumes family. The fruit is derived from hermaphrodite trees and hard in shape. The carob contains high sugar contents in pulp, fat in seed and minerals like potassium, calcium, and phosphorus are present in pods. Polyphenols and antioxidants are abundant in leaves and pods. It can be used for enhancing human health due to its high nutritional profile. Carob gum is used in the pharmaceutical industry in the form of pomades, anti-celiac ingredients, pills, and dental paste. The clinical carob can aid as an anti-cancer, anti-reflux, anti-diabetic, anti-diarrheal, anti-hyperlipidemia, anti-bacterial, anti-microbial, and anti-fungal. Nowadays, carob seeds are being used as an alternative to cocoa powder in food items whereas the leaves, pods, and seeds of carob are also historically used as food for animal feed. However, these parts of carob are available in markets with reasonable prices. Carob production, though with a rising contribution, contributes to the local economy. In this sense, we can incorporate knowledge on the chemical properties and the biological effect of carob fruits on human health. In this study, the supportive and health-promoting impacts of carob are discussed along with the clinical testing obtained from natural constituents of carob. In addition, further studies can be performed to extract and separate polyphenols and antioxidant potential for the development of functional that play a valuable role in pharmaceutical and food sectors.
Article
Introduction: Arbutus unedo L. (strawberry tree), Ceratonia siliqua L. (carob), Eucalyptus camaldulensis Dehnh. (eucalyptus), Laurus nobilis L. (laurel), Mentha aquatica L. (water mint), Myrtus communis L. (common myrtle), and Rosmarinus officinalis L. (rosemary) are aromatic plants from the Mediterranean region whose parts and preparations are used for their nutritional properties and health benefits. Objectives: To evaluate and compare the metabolites profile, total phenol content (TPC), and antioxidant activity of plant leaves for their future use. Gas chromatography-mass spectrometry (GC-MS) was used for metabolomics. Data comparison was performed by chemometrics. Methodology: Polar and apolar extracts were analysed using untargeted GC-MS metabolomics followed by chemometrics (principal component analysis, heatmap correlation and dendrogram) to identify, quantify and compare the major organic compounds in the plants. Additionally, nuclear magnetic resonance (NMR) spectroscopy was used for the laurel polar extract to identify d-gluco-l-glycero-3-octulose whose presence was unclear from the GC-MS data. TPC and antioxidant assays were performed using classical methods (Folin-Ciocalteu, 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulphonic acid) diammonium salt (ABTS), 2,2-diphenyl-1-picrylhydrazyl (DPPH)) and correlated to the phytochemical profiles. Results: Forty-three metabolites were identified including amino acids, organic acids, carbohydrates, phenols, polyols, fatty acids, and alkanes. Eight metabolites (d-fructose, d-glucose, d-mannose, gallic acid, quinic acid, myo-inositol, palmitic and stearic acids) were in common between all species. d-Gluco-l-glycero-3-octulose (37.29 ± 1.19%), d-pinitol (31.33 ± 5.12%), and arbutin (1.30 ± 0.44%,) were characteristic compounds of laurel, carob, and strawberry tree, respectively. Carob showed the highest values of TPC and antioxidant activity. Conclusion: GC-MS metabolomics and chemometrics analyses are fast and useful methods to determine and compare the metabolomics profiling of aromatic plants of food and industrial interest.
Chapter
Cyclitols are high polarity polyols, belonging to secondary metabolites, which are easily isolable from plant material. These compounds are biosynthetically derived from glucose, and occur in all living cells. They form a group of biologically active compounds and participate in many cellular processes such as: membrane biogenesis, signal transduction, ion channel physiology, osmoregulation, antioxidation, and others. The methods for the separation and determination of cyclitols include: preliminary sample preparation (drying, grinding, freezing, homogenization), sample extraction (optional: maceration, Soxhlet, ASE, MAE, SFE, UAE), isolation and purification (LLE, SPE, and others), analysis (GC-MS, HPLC, MALDI), and interpretation (identification, quantification, statistical analysis). Some other additional steps may be required, which are specific for the method chosen for the analysis. For example GC-MS analysis requires a derivatization step, while MALDI involves a laborious procedure for sample preparation. Cyclitols shows several health-promoting and therapeutic properties as follows: improving lipid profile in decreasing of serum triglycerides and total cholesterol, as well as having an insulin-mimetic effect. The beneficial properties of cyclitols are that they can be used for therapeutic purposes, particularly in neutralization of the results of chronic inflammation, which leads to increased risk of developing such metabolic disorders as diabetes, hypertension, atherosclerosis, etc. A notable factor is also good tolerance of cyclitols and their low toxicity, due to which they can be successfully used in treating pregnant women and children. Many benefits of cyclitols properties offer the possibility that these polyols may be candidates for discovery of novel drugs, food supplements and they can be used as well in cosmetic industry.
Article
The effects of hot air, microwave, and combined microwave/hot air roasting on physical and chemical properties of carob powder were determined. The comparison of different roasting processes was evaluated whether the combined microwave/hot air roasting could be an alternative to other roasting methods or not. The moisture content (2.86%–5.03%), water activity (0.20–0.35), and pH (4.94–5.12) values of the carob powder decreased by increasing microwave power and roasting time; whereas total phenolic content (10.13–13.74 mg/g dm), total antioxidant activity (0.69–1.53 g/mg DPPH), browning index (23.57–70.30), and UV absorbance (427.41–701.05) increased. Hunter L (41.54–55.28) and b (16.45–20.91) values of the carob powder decreased after roasting while color value a (8.88–20.91) increased. The main sugar was sucrose (317.54–347.68 mg/kg), followed by fructose (80.98–90.11 mg/kg), and glucose (45.16–62.19 mg/kg). Roasting process reduced the sugar content while increased the d‐pinitol (62.41–76.71 mg/kg) content. The main volatile was isobutyric acid (acidic/butter odor). Hot air and the combined microwave/hot air roasted samples showed similar volatile and sensorial profile. According to the results, the combined microwave/hot air roasting consumed 50% less energy than the hot air roasting and got the best sensory scores. The effects of microwave, hot air, and the combined microwave/hot air roasting processes on the properties of carob powder were first investigated. d‐pinitol content of carob was increased by roasting processes. Different roasting processes increased organoleptic properties of carob powder. Total phenolic content and antioxidant activity of carob powder increased by roasting. The combined microwave/hot air roasting consumed 50% less energy than the hot air roasting and it is recommended to produce carob powder with preferable product quality.
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This study investigates the effects of temperature (50–80 °C), time (10–60 min), carob-to-solvent ratio (2–8 g/40 mL), and solvent concentration (0–50 ethanol/water%, v/v) on microwave-assisted extraction of d-pinitol compound from carob fruit with optimization using Box–Behnken design. The optimal conditions for maximum d-pinitol yield (64.16 g/kg dry sample) include 50 °C temperature, 5.6 g carob/40 mL solvent, water used as a solvent, and an extraction time of 10 min. The fitness of the model was determined by ANOVA analysis with a high coefficient (R2 = 0.9057). Extraction was performed under optimum conditions for model validation, and 63.89 g/kg dry sample of d-pinitol extraction was achieved. In addition, the effects of the same variables on the total phenolic (TP) content of MEA extraction of carob were also investigated. Extraction efficiency of 426 g/kg was obtained under the optimum conditions determined for TP (80 °C, 8 g of carob, 50% ethanol, and 10 min), but it was observed that TP content decreased to 49.7 g/kg under optimum conditions determined for d-pinitol. Sucrose, glucose, and fructose sugar contents of the extract were determined only for optimum conditions for d-pinitol, and the fructose content was found to be the lowest. Determining the d-pinitol, TP, and sugar contents of the extract in optimum condition confirms the direct usability of the extract, because only water is used as a solvent. Conventional extraction method was carried out at 50 °C for control purposes, yielding 42.83 g/kg of d-pinitol, thereby supporting the effect of the microwave on extraction.
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Based on the bioactive properties of certain compounds, such as antioxidant and anti‐inflammatory activities, an interesting subject of research are natural substances present in various parts of plants. The choice of the most appropriate method for separation and quantification of biologically active compounds from plants and natural products is a crucial step of any analytical procedure. The aim of this review article is to present an overview of a comprehensive literature study from the last ten years (2007‐2017), where relevant articles exposed the latest trends and the most appropriate methods applicable for separation and quantification of biologically active compounds from plant material and natural products. Consequently, various extraction methods have been discussed, together with the available procedures for purification and pre‐concentration and dedicated methods used for analysis. This article is protected by copyright. All rights reserved
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Cyclitols are phytochemicals naturally occurring in plant material which attracted an increasing interest due to multiple medicinal attributes, amongst the most important are the anti-diabetic, antioxidant and anti-cancer properties. Due to their valuable properties, sugars are used in food industry as sweeteners, preservatives, texture modifiers, fermentation substrates, flavoring and coloring agents. In this study we report for the first time the quantitative analysis of sugars and cyclitols isolated from Solidago virgaurea L. (S. virgaurea) which was used for the selection of the optimal solvent and extraction technique that can provide the best possible yield. Moreover, the quantities of sugars and cyclitols extracted from other two species, Solidago canadensis (S. canadensis) and Solidago gigantea (S. gigantea) were investigated using the best extraction method and the most appropriate solvent. Comparative analysis of natural plant extracts obtained using five different techniques – maceration, Soxhlet extraction, pressurized liquid extraction (PLE), ultrasound assisted extraction (UAE), and supercritical fluid extraction (SFE) – was performed in order to decide the most suitable, efficient and economically convenient extraction method. Three different solvents were used. Analysis of samples has been performed by solid phase extraction (SPE) for purification and pre-concentration, followed by derivation and GC-MS analysis. The highest efficiency for the total amount of obtained compounds has been reached by PLE, when water was used as a solvent. D-pinitol amount was almost similar for every solvent and for all extraction technique involved.
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Inositol, a hexol widely found in nature with a wide range of physiological and biochemical effects, can promote fat metabolism in liver and other tissues and lower blood cholesterol and thus has been used for the clinical treatment of fatty liver, cirrhosis, atherosclerosis and hyperlipidemia. Some derivatives of inositol have been reported to have different biological activities including hypoglycemic, antitussive, anti-inflammatory and other effects. In recent years, its monomethyl ether derivatives, such as pinitol, quebrachitol, and sequoyiol, have been studied widely. In this paper, the bioactivity, extraction, preparation and applications of these monomethyl ether derivatives of inositol are reviewed. © 2014, Editorial office of Journal of International Pharmaceutical Research. All rights reserved.
Article
Ultrasound-assisted extraction (UAE) was applied to puerarin extraction from Pueraria lobata dried root to improve the extraction efficiency. By single-factor experiments, ultrasound intensity was determined at 3.0W/cm2 and the other factors (ultrasound temperature and ultrasound time) were chosen to further optimize extraction conditions using response surface methodology. The central composite experimental results showed the optimum extraction conditions as follows: an ultrasound temperature of 57.82C and an ultrasound time of 39.79min. Under these conditions, the maximal puerarin yield was 43.04mg/g. Results from the present study indicated UAE was an economical and efficient method of extracting puerarin from P.lobata dried root. Practical Applications: Puerarin can be potentially used as a healthful food additive. However, extraction efficiency of puerarin is low using traditional extraction method. This paper presents an alternative for puerarin extraction from Pueraria lobata dried root, through the development of ultrasound-assisted extraction (UAE) technology. Experimental result confirmed that UAE had many advantages compared to the traditional extraction method. On the basis of these advantages, UAE may have great potential for being scaled-up to a commercial extraction process of puerarin.
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The objective of this review is to discuss the ultrasound-assisted extraction (UAE) of various compounds using clean, green solvents. We also outline fundamental mechanisms and factors associated with the design and the development of clean, green UAE systems. Growing consumer demands for greener alternatives and natural ingredients that do not involve toxic chemicals and the environmental and health risk associated with the use of chemical solvents have attracted the interest of industries to sustainable, non-toxic routes of extraction. UAE can benefit the chemical industry in multiple ways: • enhancing extraction yield; • enhancing aqueous extraction processes without using solvents; • providing the opportunity to use alternative clean and/or green solvents by improving their extraction performance; and, • enhancing extraction of heat-sensitive components under conditions that would otherwise have low or unacceptable yields.
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An extraction method based on dispersive nanomaterial ultrasound-assisted microextraction was used for the preconcentration of carbofuran and propoxur insecticides in water samples prior to high-performance liquid chromatography with UV detection. ZnS:Ni nanoparticles were synthesized based on the reaction of the mixture of zinc acetate and nickel acetate with thioacetamide in aqueous media and then loaded on activated carbon (ZnS:Ni-AC). Different methods were used for recognizing the properties of ZnS:Ni-AC and then this nanomaterial was used for extraction of carbamate insecticide as new adsorbent. The influence of variables on the extraction method (such as amount of adsorbent (mg: NiZnS-AC), pH and ionic strength of sample solution, vortex and ultrasonic time (min), ultrasound temperature and desorption volume (mL) was investigated by a screening 27–4 Plackett–Burman design. Then the significant variables were optimized by using a central composite design combined with a desirability function. At optimum conditions, this method had linear response >0.0060–10 μg/mL with detection limit 0.0015 μg/mL and relative standard deviations <5.0% (n = 3).
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Pods and seeds from carob Ceratonia siliqua L. trees growing in Ajloun Mountainous forests and rangelands in Jordan were analyzed for their proximate analysis, Ca and P contents, and also the effects of ingestion of seeds by sheep and goat on the germination were investigated. Carob seed has hard seed coat dormancy, and seed scarification increased germination from 10.2% in non-scarified to 85.4% after scarification. Germination percentages for seeds that were ingested by sheep were 73.5, 61.8, 39.3, and 0.0% for ingestion periods of 24, 48, 72, and 96 hours, respectively; whereas, it was 56.8, 79.9, 50.1, 13.7, and 1.1 % for seeds dispersed from goat after 24, 48, 72, 96, and 120 hours. Carob seeds contained higher amounts of protein, fiber, fat and Ca. than deseeded pods. However, the latter contained more carbohydrates and P than seeds. Carob pods and seeds contained sufficient crude protein and energy to meet the maintenance and lactation requirements of ewes, but Ca and P contents were not adequate by themselves.
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Total mass transfer coefficients of soluble solids (SS) and total phenolic compounds (TPC) were determined during carob extraction. The Arrhenius equation was applied to determine the efficiency of process temperature, as an alternative approach to Fick's second law. Carob pod, cut into small pieces (internal diameter: 5–7 mm), was contacted with water in batch system to extract SS by continuous circulation of water at different temperatures (20, 50 and 85C). The process was also performed at 85C using an industrial-scale extractor. Activation energies for both SS and TPC diffusions were calculated as 5.84 and 0.072 × 10−3 kJ/mol, respectively. As expected, higher extract concentrations were achieved with higher temperatures. In contrast, high extraction temperature, even at 85C, did not cause hydroxymethylfurfural (HMF) formation. As the increase in temperature does not affect formation of HMF during carob pod extraction, higher operational temperatures such as 80–90C may be applied to obtain higher solute concentrations.
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Hawthorn seed (HS), an important by-product of the Hawthorn industry, is rich in potentially health-promoting flavonoids compounds. In this paper, the ultrasound-assisted extraction (UAE) of FC from HS was investigated. Important variables and their levels were obtained using Plackett-Burman (PB) design and Box-Behnken (BB) design. A mathematical model was developed to show the effects of each variable and their combinatorial interactions on extraction yield of FC. A high coefficient of determination (R(2) = 91.26%) indicated good agreement between the experimental and predicted values of FC yield. The optimum levels of these significant parameters were determined using response surface methodology (RSM), which revealed these as follows: ultrasound temperature 65 °C, ultrasonic time 37 min, extraction temperature 91 °C, extraction time 1.5h, solid-liquid ratio of 1:18, and 72% ethanol. Under the optimum condition, the UAE rate of FC was up to 91.7%, and the yield of FC was 16.45 ± 0.02 mg/g (P<0.05) that was 1.32-fold the yield of conventional reflux extraction (CRE).
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Bamboo was submitted to ultrasound-assisted extraction in aqueous ethanol to evaluate the effect of ultrasonic irradiation on the dissolution of lignin. In this case, the dewaxed bamboo culms were subjected to ball milling for 48 h, and then were suspended in 95% ethanol followed by ultrasonic irradiations for varied times at 20 °C to obtain ethanol-soluble fractions. The structural and thermal properties of the ethanol-soluble fractions were comparatively investigated by chemical analysis including alkaline nitrobenzene oxidation, bound carbohydrate determination, FT-IR spectra, HSQC spectra, TG, and DTA. The results showed that the yields of the ethanol-soluble fractions were between 4.29% and 4.76% for the fractions prepared with ultrasonic irradiation time ranging from 5 to 55 min, as compared to 4.02% for the fraction prepared without ultrasonic irradiation. It was found that the lignin content of the fraction increased with the increase of the ultrasonic irradiation time. There was a slight increase of the molecular weight of the lignin with the increase of the ultrasonic irradiation time. Alkaline nitrobenzene oxidation coupled with HSQC analysis indicated that the lignin in the fractions was mainly composed of GSH type units as well as minor amounts of ferulic acids. In addition, the fraction prepared with ultrasonic irradiation exhibited a slightly higher thermal stability as compared to the fraction prepared without ultrasonic irradiation.
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Lycopene extraction was carried out via the ultrasonic assisted extraction (UAE) with response surface methodology (RSM). Sonication enhanced the efficiency of relative lycopene yield (enhancement of 26% extraction yield of lycopene in 6 replications at 40.0 min, 40.0 °C and 70.0% v/w in the presence of ultrasound), lowered the extraction temperature and shortened the total extraction time. The extraction was applied with the addition of oxygen-free nitrogen flow and change of water route during water bath sonication. The highest relative yield of lycopene obtained was 100% at 45.0 °C with total extraction time of 50.0 min (30:10:10) and ratio of solvent to freeze-dried tomato sample (v/w) of 80.0:1. Optimisation of the lycopene extraction had been performed, giving the average relative lycopene yield of 99% at 45.6 min, 47.6 °C and ratio of solvent to freeze-dried tomato sample (v/w) of 74.4:1. From the optimised model, the average yield of all-trans lycopene obtained was 5.11±0.27 mg/g dry weight. The all-trans lycopene obtained from the high-performance liquid chromatography (HPLC) chromatograms was 96.81±0.81% with 3.19±0.81% of cis-lycopenes. The purity of total-lycopene obtained was 98.27±0.52% with β-carotene constituted 1.73±0.52% of the extract. The current improved, UAE of lycopene from tomatoes with the aid of RSM also enhanced the extraction yield of trans-lycopene by 75.93% compared to optimised conventional method of extraction. Hence, the current, improved UAE of lycopene promotes the extraction yield of lycopene and at the same time, minimises the degradation and isomerisation of lycopene.
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To assess the effects of soybean-derived pinitol on glycaemic control and cardiovascular risk factors in Korean patients with type II diabetes mellitus. Randomized, double-blind, placebo-controlled, parallel-group trial. Pusan Paik Hospital, Pusan, Republic of Korea. A total of 30 patients with type II diabetes received an oral dose of 600 mg soybean-derived pinitol or placebo twice daily for 13 weeks. Pinitol significantly decreased mean fasting plasma glucose, insulin, fructosamine, HbA1c, and the homeostatic model assessment insulin resistance index (HOMA-IR, P<0.001). Pinitol significantly decreased total cholesterol, LDL-cholesterol, the LDL/HDL-cholesterol ratio, and systolic and diastolic blood pressure and increased HDL-cholesterol (P<0.05). These data suggest that soybean-derived pinitol may be beneficial in reducing cardiovascular risk in Korean type II diabetes.
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Carob syrup is a traditional product native to the Mediterranean region, containing a high concentration of sugar, phenolic compounds and minerals. d-pinitol is a bioactive component extracted from legumes and has some beneficial effects on human metabolism. In this research, the d-pinitol content and sugar profile of 10 different carob syrup samples purchased from Turkish markets were determined. Mean d-pinitol, sucrose, glucose and fructose contents of samples were found to be 84.63 ± 10.73, 385.90 ± 45.07, 152.44 ± 21.72 and 162.03 ± 21.45 g/kg dry weight, respectively. Carob syrup has a considerable amount of d-pinitol compared with the other d-pinitol-including legumes. Consequently, this study showed that carob syrup may be a suitable source of d-pinitol for medical use and d-pinitol may be an indicator for the detection of any adulteration in carob syrup.
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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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d-chiro-Inositol (DCI) is a drug candidate for the treatment of type 2 diabetes and polycystic ovary syndrome, since it improves the efficiency with which the body uses insulin and also promotes ovulation. Here, we report genetic modification of Bacillus subtilis for production of DCI from myo-inositol (MI). The B. subtilis iolABCDEFGHIJ operon encodes enzymes for the multiple steps of the MI catabolic pathway. In the first and second steps, MI is converted to 2-keto-MI (2KMI) by IolG and then to 3d-(3,5/4)-trihydroxycyclohexane-1,2-dione by IolE. In this study, we identified iolI encoding inosose isomerase, which converts 2KMI to 1-keto-d-chiro-inositol (1KDCI), and found that IolG reduces 1KDCI to DCI. Inactivation of iolE in a mutant constitutively expressing the iol operon blocked the MI catabolic pathway to accumulate 2KMI, which was converted to DCI via the activity of IolI and IolG. The mutant was able to convert at least 6% of input MI in the culture medium to DCI.
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The effect of 3-O-methyl-D-chiro-inositol (D-pinitol), purified from soybean, on the postprandial blood glucose response in patients with type 2 diabetes mellitus was examined. Fifteen Korean subjects with type 2 diabetes mellitus (seven men, eight women; 60.3 +/- 3.1 years old) ingested cooked white rice containing 50 g of available carbohydrate with or without prior ingestion of soy pinitol. Pinitol was given either as a 1.2 g dose at 0, 60, 120, or 180 minutes prior to rice ingestion, or as a 0.6 g dose at 60 minutes prior to rice ingestion. Capillary blood glucose levels were monitored for 4 hours after rice consumption. The ingestion of 1.2 g of pinitol 60 minutes prior to rice consumption controlled postprandial capillary blood glucose most effectively, significantly diminishing the postprandial increase in plasma glucose levels measured at 90 and 120 minutes after rice consumption (P < .05). The incremental area under the plasma glucose response curve for subjects who consumed both pinitol and rice was significantly lower than that for subjects who consumed only rice (P < .05), but pinitol had no apparent effect on postprandial insulin levels. Therefore, soybean-derived pinitol may be useful in controlling postprandial increases in blood glucose in patients with type 2 diabetes.
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Hesperidin, an abundant and inexpensive bioflavonoid in Penggan (Citrus reticulata) peel, has been reported to possess a wide range of pharmacological properties. Ultrasonic extraction is an effective technique for the isolation of bioactive compounds from vegetable materials. In this study, the application of ultrasonic method was shown to be more efficient in extracting hesperidin from Penggan (C. reticulata) peel than the classical method. The effects of main ultrasonic-assisted extraction conditions on extraction yields of hesperidin from Penggan (C. reticulata) peel were evaluated, including extraction solvents, solvent volume, temperature, extraction time, ultrasonic power, ultrasonic frequency. Results showed that solvent, frequency and processing temperature were the most important factors for improving the extracting yields of hesperidin. When performed at the same temperature under the same time using three frequencies, methanol as the solvent improved the extraction yield evidently compared with ethanol or isopropanol; by comparison of the frequency influence, the yield of hesperidin was higher at 60 kHz than at 20 kHz and 100 kHz. The optimum ultrasonic conditions were determined as: methanol, frequency of 60 kHz, extraction time of 60 min, and temperature of 40 degrees C. In addition, the ultrasonic power had a weak effect on the yields of hesperidin within the experimental range. Extending ultrasonic treatment times did not result in degradation of hesperidin; the rotary beaker for materials can increase the yields of hesperidin.
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Various two-step extraction procedures with and without a short application of ultrasound in the first step at various reaction conditions (extracting agent, temperature and time), and constant conditions in the second step (5% NaOH, room temperature, 60 min) were used to isolate the hemicellulose component of industrial wheat bran. The polysaccharides recovered from the extracts were characterised by yield, chemical composition and radical scavenging activity. Similar total yields of polysaccharides were achieved by a short ultrasound-assisted extraction (up to 10 min) in the first step using 0.5% or 2% NaOH, when compared to the classical extraction lasting 60 min, what represents a shortening of the process by about 60% and lower consumption of the NaOH. The extracted polysaccharides comprised a complex of phenolics-rich heteroxylans contaminated to various extents with co-extracted amylose-rich starch as well as protein, which can be in part governed by the extraction conditions. The water-soluble fractions from both the classical and ultrasonics experiments were shown to exhibit significant radical scavenging activity in vitro, indicating their potential application as polysaccharide-based antioxidants.
Article
The carob pod, an important fruit of the food industry in the production of concentrated syrup, is rich in potentially health-promoting phenolic compounds and sugars. Moreover, one of the important bioactive components of carob is D-pinitol, and it has some beneficial effects on human metabolism. The optimum conditions for extraction of D-pinitol and total phenolic compounds (TPC) from cultivated and wild types of carob pods were determined using response surface methodology (RSM). The Box-Behnken Design (BBD) was used to investigate the effects of three independent variables; extraction temperature (degrees C), dilution rate (w/v), and extraction time (h) on the response, D-pinitol and the total phenolic compounds. The optimum extraction conditions obtained using the response optimizer were an extraction temperature of 80 degrees C, a dilution rate of 1:4, and an extraction time of 2h. Under the mentioned above conditions, the maximum D-pinitol and TPC concentrations were 9.67 g/L and 5916.55 mg/L in wild carob pod extract, respectively.
Article
Microwave-assisted Extraction (MAE) and Ultrasound-assisted extraction (UAE) techniques have been employed as complementary methods to extract carbohydrates, polysaccharides and other functional compounds from vegetable sources. In this work, the effect of microwave power and heating time on the yield and quality of extracted pectin from grapefruit was investigated. The highest total amount of pectin yield was found to be 27.81% (w/w) for 6min of extraction at 900W. It was observed that yield, the galacturonic acid content (GalA), and degree of esterification (DE) increased with an increase in microwave power and heating time. Besides, the molecular weight decreased with an increase in heating time; however, the effects of power on the molecular weight were dramatically more than heating time. In addition, laboratory studies on the extraction of pectin treated with high-intensity ultrasound were carried out. The effects of temperature and time on quality and quantity of extracted pectin were investigated. The highest yield was for sonication time of 25min (17.92%) in a constant bath temperature of 70°C. Furthermore, a preliminary ultrasonic heating of grapefruit solution, as a pretreatment for MAE, was found to provide a higher yield. Intermittent sonication gave better results in comparison to the continuous sonication.
Article
There is growing interest in the use of D-pinitol (D-3-O-methyl-chiro-inositol) as a food supplement because of its reported efficacy in lowering blood glucose levels. Pinitol is a common constituent of legume plants and is a major component of soybean [Glycine max (L.) Merr.] leaves. The objective of the studies was to identify a combination of simple methods that would result in the purification of pinitol from soybean leaves. Ethanolic extracts of soybean leaves following solvent partitioning to remove lipids, passage of the aqueous fraction through ion exchange resins, and treatment of the effluent with activated charcoal yielded a white crystalline product that was 85.5% pinitol by weight. Other components in the product included D-chiro-inositol (5.2%), myo-inositol (3.4%), and ononitol (D-4-O-methyl-myo-inositol; 1.9%). Thus, 96% of the crystalline product was cyclitols following the simple purification protocol.
Article
Available archaeo-botanical finds (most of them from Israel) show that the carob Ceratonia siliqua L. existed in the Eastern Mediterranean basin long before the start of agriculture. Early literary sources indicate that its domestication took place relatively late (only in Roman times). The probable reason for this late date is that the carob does not lend itself to simple vegetative propagation, and its cultivation had to wait until the introduction of scion grafting into the Mediterranean basin. Carob culture reached its peak in this region in early Islamic times. C. siliqua cultivars and wild-growing trees frequently grow side by side, and intercross rather freely. It is proposed that under domestication, hermaphroditic clones were favored, causing a partial breakdown of dioecy in carob culture. Through introgression, this development also affected some of the wild populations.
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Carob pods contain about 200–500 g/kg of total sugars, a higher content of sugar than is present in beet or cane, which is below 200 g/kg. In the present paper a sugar syrup (concentrate solution of several sugars) from carob pods has been obtained with a concentration of sugars near 580 g/kg, 62° Brix and 93% of purity. Extraction and purification techniques were performed. From the results of the extraction researches it can be concluded that a 10 column system connected in series is the most advantageous for efficiency and automation of the sugar extraction reaching a yield of at least 90%. In the purification technique a discontinuous treatment followed by purification in several types of columns connected in series have been studied in order to obtain a transparent and colourless extract.
Article
Carob has been widely grown in the Mediterranean region for centuries. It has been regarded as only a forest tree and has been neglected for other economical benefits. However, in recent years, it has gained attention for several applications. In this study, carob extract has been used as carbon source in fermentation. Lactic acid is considered to be an industrial chemical used in food, textile and pharmaceutical industries. Lactic acid demand has recently increased because of its role as a monomer in the production of biodegradable polylactic acid (PLA), which is known as a sustainable and degradable bioplastic material. Therefore, this study was undertaken to evaluate the potential of carob extract for lactic acid production. Based on our previous study, the optimum extraction conditions were used to obtain the carob extract with high sugar content. Then, obtained extract was utilized by Lactobacillus casei for production of lactic acid by using suspended-cell fermentation. Although carob pod contains 40–50% sugars (especially, sucrose), L. casei could not metabolize them in this complex form. Therefore, sucrose in extract was converted into the monosaccharides by using invertase enzyme prior to fermentation. Also, in order to determine economical appropriate nitrogen sources, four different nitrogen sources were evaluated. The maximum lactic acid concentration and yield for carob extract with yeast extract was 31.35 (g/L) and 68.79% compared with 59.27 (g/L) and 66.70% after using invertase enzyme. Results clearly showed that carob pods can be a good feedstock for lactic acid production by L. casei.
Article
In the food industry, carob powder is used as a cocoa substitute. It consists primarily of sugars (sucrose, glucose, fructose) in addition to tannins, fibers, etc. D-(+)-Pinitol (3-O-methyl-D-chiro-inositol), myo-inositol, and D-(+)-chiro-inositol were isolated from a fermented water extract of carob powder. The concentration of pinitol ranged from 5 to 7.5% of the dry weight of the powder as determined by GC. myo-Inositol and chiro-inositol were minor components with concentrations of 0.5 to 1% and 0.1%, respectively. As pinitol is not present in cocoa powder, it can be used as a natural marker of carob adulteration of cocoa powder. Further investigations, including GC-MS, revealed traces of ononitol (4-O-methyl-myo-mositol), sequoyitol (5-O-methyl-myo-inositol), and bornesitol (1-O-methyl-myo-inositol) to be present in a fermented water extract of carob powder in addition to sorbitol.
Article
The aim of the study was to determine the main sugar profiles of the pods, without the seeds, of cultivated and wild types of the carob bean grown in the Mediterranean and Aegean basin of Turkey. The most abundant sugar in the pods was sucrose with smaller amounts of glucose and fructose. The pods of cultivated varieties had a higher (p < 0.05) total sugar concentration of 531 ± 93 g/kg dry weight than the wild type selections which had 437 ± 77 g/kg. However, this difference was due to the greater concentration of sucrose in the cultivated varieties which did not differ from the wild types in their concentrations of fructose or glucose. The ratios of individual sugars to total sugars in the pods were similar in both varieties. There is a need to identify extreme wild types, including high seeds and low pod, and cultivated types, containing low seeds and high pod, rich in sugar for an exhaustive picture of the sugar profiles of the varieties.
Article
The research was carried out to evaluate gelling and bleaching agents for white solid pekmez production. Grape juice with 26% total soluble solids as °Brix was used for the production of pekmez. Acidity was reduced with the application of sterile white soil containing 70.4% CaCO3, followed by tannin–gelatin clarification and filtration. The grape juice was concentrated to 76% total soluble solids by vacuum. Gelling treatments were designed to produce a solid pekmez by adding high or low methoxyl pectins or carboxymethylcellulose (CMC). It was found that sufficient gelling could be achieved using less than 0.5% CMC and 1% for either pectin. Also, a desirable white color was obtained with 1.5% soapwort juice and 3% egg white with the combination of 1% pectins.
Article
Ultrasound-assisted extraction (USAE) is an interesting process to obtain high valuable compounds and could contribute to the increase in the value of some food by-products when used as sources of natural compounds. The main benefits will be a more effective extraction, thus saving energy, and also the use of moderate temperatures, which is beneficial for heat-sensitive compounds. For a successful application of the USAE, it is necessary to consider the influence of several process variables, the main ones being the applied ultrasonic power, the frequency, the extraction temperature, the reactor characteristics, and the solvent–sample interaction. The highest extraction rate is usually achieved in the first few minutes, which is the most profitable period. To optimize the process, rate equations and unambiguous process characterization are needed, aspects that have often been lacking.
Article
Oxidative stress plays a crucial role in the progression and development of diabetes and its complications due to chronic hyperglycemia. The present study was aimed to investigate the kidney tissue protective nature of d-pinitol, a cyclitol present in soybean, by assessing the key markers of hyperglycemia-mediated oxidative stress, proinflammatory cytokines and ultrastructural alterations in streptozotocin-induced diabetic rats. Oral administration of d-pinitol (50mg/kg body weight/day) for 30 days to diabetic group of rats showed a significant elevation in the level of total protein and significant decline in the levels of blood urea, serum uric acid, creatinine and advanced glycation endproducts (AGEs) and kidney proinflammatory cytokines such as TNF-alpha, IL-1beta, IL-6, NF-kappaB p65 subunit and nitrite. Further, d-pinitol administration elicited a significant attenuation in the activities of kidney enzymatic antioxidants such as superoxide dismutase (SOD), catalase, glutathione peroxidase (GPx), glutathione-S-transferase (GST) and glutathione reductase (GR) and the levels of kidney non-enzymatic antioxidants such as vitamin E, vitamin C and reduced glutathione (GSH) in the diabetic group of rats, with a concomitant decline in the levels of kidney lipid peroxides, hydroperoxides and protein carbonyls. The histological and ultrastructural observations on the kidney tissues also confirmed the renoprotective nature of d-pinitol. Thus the present study demonstrated the renoprotective nature of d-pinitol by attenuating the hyperglycemia-mediated proinflammatory cytokines and antioxidant competence in kidney tissues of streptozotocin-induced diabetic rats.
Article
Carob has been widely grown in the Mediterranean region for a long time. It has been regarded as only a forest tree and has been neglected for other economical benefits. However, in recent years, this fruit has gained attention for several applications. As petroleum has become depleted, renewable energy production has started to gain attention all over the world; including the production of ethanol from underutilized agricultural products such as carob. In this project, the optimum extraction conditions were determined for the carob fruit by using the response surface design method. The obtained extract was utilized for production of ethanol by using suspended Saccharomyces cerevisiae fermentation. The effect of various fermentation parameters such as pH, media content and inoculum size were evaluated for ethanol fermentation in carob extract. Also, in order to determine economically appropriate nitrogen sources, four different nitrogen sources were evaluated. The optimum extraction condition for carob extract was determined to be 80 degrees C, 2h in 1:4 dilution rate (fruit: water ratio) according to the result of response surface analysis (115.3g/L). When the fermentation with pH at 5.5 was applied, the final ethanol concentration and production rates were 42.6g/L and 3.37 g/L/h, respectively, which were higher than using an uncontrolled pH. Among inoculum sizes of 1%, 3%, and 5%, 3% was determined as the best inoculum size. The maximum production rate and final ethanol concentration were 3.48 g/L/h and 44.51%, respectively, with an alternative nitrogen source of meat-bone meal. Overall, this study suggested that carob extract can be utilized for production of ethanol in order to meet the demands of renewable energy.
Article
This study was performed to investigate the lipid-lowering, antioxidant, and hepato-protective effects of pinitol in dose-dependent manners in hamsters fed-high fat and high cholesterol (HFHC) diet. Pinitol supplementation (0.05%, P-I and 0.1% pinitol, P-II) with an HFHC diet (10% coconut oil plus 0.2% cholesterol) for 10 wks significantly lowered the white adipose tissue weights, hepatic lipid droplets, plasma glucose, total-cholesterol, nonHDL-cholesterol, total-cholesterol/HDL-cholesterol ratio, and hepatic lipid levels. Whereas it significantly increased the brown adipose tissue weight, plasma HDL-cholesterol, apolipoprotein A-I (apo A-I) concentrations, paraoxonase (PON) activity, and/or mRNA expression, compared to the HFHC control group. Plasma insulin and adiponectin levels were significantly lower and higher, respectively, in both P-I and P-II groups than the HFHC control group. Dietary pinitol significantly inhibited hepatic HMG-CoA reductase, acyl-CoA:cholesterol acyltransferase (ACAT), and cytochrome P4502E1 (CYP2E1) activities without altering their mRNA expressions compared to the control group. Pinitol significantly elevated the hepatic antioxidant enzyme activities, whereas it also significantly reduced the hepatic lipid peroxide and H2O2 production. Accordingly, these results indicate that both 0.05 and 0.1% pinitol supplementation may improve the lipid and antioxidant metabolism in HFHC diet-fed hamsters. In particular, pinitol supplementation was very effective on the elevation of antiatherogenic factors, including plasma HDL-cholesterol, apo A-I, adiponectin, and PON.
Article
D-pinitol (3-O-methyl-chiroinositol), an active principle of the traditional antidiabetic plant, Bougainvillea spectabilis, is claimed to exert insulin-like effects. This study was undertaken to evaluate the effect of D-pinitol on lipids and lipoproteins in streptozotocin (STZ)-induced diabetic Wistar rats. Rats were made type II diabetic by single intraperitoneal injection of STZ at a dose of 40 mg/kg body weight. STZ-induced diabetic rats showed significant (p < 0.05) increase in the levels of blood glucose and total cholesterol, triglycerides, free fatty acids, and phospholipids in serum, liver, kidney, heart, and brain. The levels of low-density lipoprotein (LDL) and very low-density lipoprotein (VLDL) cholesterol were significantly increased, and the level of high-density lipoprotein (HDL) cholesterol was significantly decreased in diabetic rats Oral administration of D-pinitol to STZ-induced diabetic rats showed significant (p < 0.05) decrease in the levels of blood glucose and total cholesterol, triglycerides, free fatty acids, and phospholipids in serum, liver, kidney, heart, and brain. The D-pinitol also lowered significantly (p < 0.05) LDL and VLDL cholesterol levels and increased significantly (p < 0.05) HDL cholesterol levels in the serum of diabetic rats. Thus, the present study clearly showed the antihyperlipidemic effect of D-pinitol in STZ-induced type II diabetic rats.
Article
The production of citric acid from carob pod extract by A. niger in surface fermentation was investigated. A maximum citric acid concentration (85.5 g/L), citric acid productivity (4.07 g/L/d), specific citric acid production rate (0.18 g/g/d), and specific sugar uptake rate (0.358 g/g/d) was achieved at an initial sugar concentration of 200 g/L, pH of 6.5, and a temperature of 30 degrees C. Other kinetic parameters, namely, citric acid yield, biomass yield, specific biomass production rate, and fermentation efficiency were maximum at pH 6.5, temperature 30 degrees C, and initial sugar concentration 100 g/L. The external addition of methanol into the carob pod extract at a concentration up to 4% (v/v) improved the production of citric acid.
Article
D-pinitol (3-O-methyl-chiroinositol), an active principle of the traditional antidiabetic plant Bougainvillea spectabilis, is claimed to exert insulin-like effects. This study investigates the effect of D-pinitol on glucose homeostasis in animal models of diabetes, and on glucose transport by cultured muscle cells. Plasma glucose concentrations were measured in normal, obese-diabetic (ob/ob) and streptozotocin (STZ)-diabetic mice after oral (p.o.) and intraperitoneal (i.p.) administration of D-pinitol. Glucose transport was measured in L6 rat muscle cells by 2-deoxyglucose (2DG) uptake. In STZ-diabetic mice, 100 mg kg−1 p.o. D-pinitol acutely decreased the hyperglycaemia (by 22% at 6 h). A similar decrease in plasma glucose (by 21%) was observed after 100 mg kg−1 i.p. D-pinitol. Insulin concentrations and the rate of insulin-induced (1 unit kg−1 actrapid i.p.) glucose disappearance were not altered by 100 mg kg−1 p.o. D-pinitol. Chronic administration of D-pinitol (100 mg kg−1 i.p. twice daily for 11 days) to STZ-diabetic mice maintained a reduction in plasma glucose concentrations from about 14 to 10 mmol l−1. In normal non-diabetic and severely insulin resistant ob/ob mice, 100 mg kg−1 p.o. D-pinitol did not significantly affect plasma glucose or insulin during acute studies. Incubation of L6 muscle cells with D-pinitol (10−3 M) increased basal 2DG uptake by 41% after 10 min and by 34% after 4 h. The effect of D-pinitol was inhibited by the phosphatidylinositol 3-kinase inhibitor LY294002. D-pinitol did not increase insulin-stimulated 2DG uptake by L6 cells. The data support the view that D-pinitol can exert an insulin-like effect to improve glycaemic control in hypoinsulinaemic STZ-diabetic mice. D-pinitol may act via a post-receptor pathway of insulin action affecting glucose uptake. British Journal of Pharmacology (2000) 130, 1944–1948; doi:10.1038/sj.bjp.0703523
Article
In the carrageenin-induced paw oedema in rats, (+)-pinitol (2.5-10 mg/kg, i.p.), isolated from Abies pindrow leaves, showed a significant anti-inflammatory effect, the highest dose being comparable to phenylbutazone (100 mg/kg, i.p.).
Article
The insoluble plant residues, obtained after preparation of medicinal tinctures from the roots of valerian (Valeriana officinalis L.) by classical and ultrasound-assisted extraction with aqueous ethanol in a pilot plant, were subsequently treated with hot water to isolate the accessible polysaccharide cell wall components. At almost equal amounts of the hot-water extractable material, the yields of the recovered polysaccharides were lower in the ultrasonical experiment. This is due to the fact that a part of accessible polysaccharides were already solubilised by the aqueous ethanol and recoverable from the medicinal tincture. Therefore, the net yield of extracted polysaccharides was enhanced in the ultrasonical procedure. This fact as well as the sugar composition and structural features of the isolated polysaccharides suggest that ultrasonication have attacked the integrity of cell walls, released and degraded its most accessible polysaccharides (pectic polysaccharides and starch) and increased also the extractibility of its less accessible components--xylan, mannan and glucan. The water-soluble polysaccharide fractions from both the conventional and ultrasonical experiments exhibit significant immunostimulatory activities in mitogenic and comitogenic thymocyte tests.
Article
Ultrasound-assisted extraction was evaluated as a simpler and more effective alternative to conventional extraction method for the isolation of xyloglucan from apple pomace. The apple pomace samples were extracted under indirect sonication in an ultrasound cleaning bath. The ultrasound extraction was compared with the conventional method, on the productions of xyloglucan. It was found that the ultrasound-assisted extraction of xyloglucan was about three times faster than the traditional extraction method. Response surface methodology was employed to study the effect of liquid:solid ratio, KOH concentration and ultrasound-assisted extraction time on the yield of xyloglucan from apple pomace. Regression analysis was performed on the data obtained. The most relevant variable was the quadratic of liquid:solid ratio. The coefficient determination (R(2)) was good for the second-order model. The optimum combination was determined as a liquid:solid ratio of 34.4:1 (v/w), a KOH concentration of 3.3 M and an ultrasound-assisted extraction time of 2.5 h.
Article
Pinitol (3-O-methyl-D-chiro-inositol) was identified in putative insulin mediator fractions that have hypoglycemic activity, and appears to mimic the act effects of insulin by acting downstream in the insulin signaling pathway. We evaluated the effect of pinitol therapy in type 2 diabetic patients who were poorly controlled with hypoglycemic drugs, such as sulfonylurea, metformin and/or insulin. Twenty type 2 diabetic patients were enrolled in our study. Fasting glucose, fasting c-peptide, total cholesterol, triglyceride, and HDL- and LDL-cholesterol were checked before and after a 12-week pinitol treatment (20 mg kg(-1)day(-1)). All subjects continued their current medications during the study. Adipocytokines, such as adiponectin, leptin, free fatty acids, and c-reactive protein (CRP) were checked before and after pinitol treatment. After pinitol treatment, fasting glucose, post-prandial glucose levels, and hemoglobin A1c were significantly decreased (P<0.05). Fasting serum adiponectin, leptin, free fatty acid, and CRP levels did not change after pinitol treatment. In the unresponsive group, serum c-peptide levels were higher than in the responsive group. Twelve weeks of pinitol treatment altered glucose metabolism, but not lipid profiles or adipocytokine levels, in type 2 diabetic patients. Additional research is needed to define the physiological and potential therapeutic effects of pinitol administration.
The effect of pinitol on cataractogenesis in streptozotocin induced diabetic rats
  • J Park
  • Y Lee
  • J Kim
  • Y Shin
  • J Kim
J. Park, Y. Lee, J. Kim, Y. Shin, J. Kim, The effect of pinitol on cataractogenesis in streptozotocin induced diabetic rats, Invest. Ophth. Vis. Sci. 45 (2004) U606.
Use of pinitol or chiroinositol for protecting the liver
  • Y C Shin
  • Y J Jeon
  • J J Kim
Y.C. Shin, Y.J. Jeon, J.J. Kim, Use of pinitol or chiroinositol for protecting the liver, in, Google Patents, 2004.
Analytical applications of ultrasound, in: techniques and instrumentation in analytical chemistry
  • M D Luque De Castro
  • F Priego-Capote
M.D. Luque de Castro, F. Priego-Capote, Analytical applications of ultrasound, in: techniques and instrumentation in analytical chemistry, Elsevier, Amsterdam, The Netherlands, 2006. p. 350.
The effect of pinitol on cataractogenesis in streptozotocin induced diabetic rats
  • Park