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Extraction of vanillin from vanilla pods: A comparison study of conventional soxhlet and ultrasound assisted extraction

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Abstract

This study deals with extraction of vanillin from cured vanilla pods using conventional soxhlet extraction and ultrasound assisted extraction. Effect of various extraction parameters such as type of the solvent (6 different solvents viz. ethanol, methanol, acetonitrile, acetone, chloroform and hexane), quantity of beans (1–3g), operating temperature (in the range 90–100°C) for soxhlet extraction and pre-leaching time (in the range of 30–90min) for ultrasound assisted extraction, on the extent of extracted vanillin has been investigated in this work. It has been conclusively established that the use of polar solvents resulted in maximum extent of extraction for both the types of extraction operations. For soxhlet extraction, an increase in operating temperature from 90°C to 100°C was found to increase extent of extraction by 30% whereas for ultrasound assisted extraction, pre-leaching stage for 30min duration was found to be beneficial in enhancing the extent of extraction by about 20%. The use of ultrasonic irradiation resulted in intensification of the extraction operation of vanillin significantly as confirmed from the results that in soxhlet extraction, an operating temperature of 95°C and solvent to solute proportion of 66.67ml/g (most commonly used conditions) resulted in release of around 180ppm in 8h whereas ultrasonic assisted extraction required only 1h for release of around 140ppm vanillin concentration at similar proportions of solvent to solute and under ambient operating temperature.

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... The volume of ethyl acetate added was thought to affect the levels of vanillin produced. Jadhav et al. (2009) showed that vanillin extraction from vanilla beans gave the lowest yield at a solvent volume of 66.67 ml and increased by about 50% at 100 ml solvent volume, but only slightly increased at 200 ml solvent volume. The volume of solvent used in the extraction process is critical in the production of vanillin compounds (Dağdelen & Dağdelen, 2016). ...
... However, the vanillin yield tends to decrease at a certain limit point because the solvent has reached its saturation point and is considered the optimal point. According to Jadhav et al. (2009), the extraction rate almost follows a linear path with extraction time and will decrease with longer extraction time. Table 3 shows that the highest vanillin yield was in the extraction of degraded OPEFB using Serpula lacrymans of 7.778 µg/g in the combination treatment of adding 100 ml volume of ethyl acetate with an extraction time of 120 minutes. ...
... It is assumed that due to the polarity of the solvent, the extraction will increase with the increasing polarity of the solvent. In the research of Jadhav et al. (2009), the optimal solvent volume for vanillin extraction is 100 ml. The solvent takes a particular time to enter between the matrices by breaking the matrix so that the compounds in the material will come out (Dong et al., 2014). ...
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This research aims to determine the combination of the ethyl acetate solvent volume and the extraction time that resulted in the optimum response of vanillin content and vanillin yield from the degradation of lignocellulose components from oil palm empty fruit bunches (OPEFB). First, OPEFB degraded using Serpula lacrymans to break down lignocellulosic components. The research design used a centralized composite design with two factors, the volume of ethyl acetate solvent (ml) and the extraction time (minutes). The responses of the experiment are vanillin content and vanillin yields. The optimization analysis results showed that the volume of ethyl acetate solvent and extraction time have a quadratic effect on the vanillin content and vanillin yields. The optimal solution was obtained by treatment with ethyl acetate volume 101.1 ml and extraction time 123.5 minutes. The optimal solution prediction results obtained vanillin content 0.014% and vanillin yield 7.302 μg/g with desirability of 92.8%. Validation based on the optimal solution’s prediction brought response vanillin content 0.013% and vanillin yield 6.950 μg/g. The vanillin content and yield validation results differed respectively by 4.081% and 4.826% lower when compared to predictions on the optimal solution. Keywords: ethyl acetate, vanillin content, vanillin yield Abstrak Penelitian ini bertujuan untuk mengetahui kombinasi dari volume pelarut etil asetat dan lama waktu ektraksi yang menghasilkan respon kadar vanillin dan yield vanillin optimum dari hasil degradasi komponen lignoselulosa tandan kosong kelapa sawit. Tandan kosong kelapa sawit terlebih dahulu didegradasi menggunakan jamur pelapuk Serpula lacrymans untuk memecah komponen lignoselulosa. Rancangan penelitian menggunakan rancangan komposit terpusat dengan dua faktor, yaitu volume pelarut etil asetat (ml) dan lama waktu ekstraksi (menit). Respon dari percobaan tersebut adalah kadar vanillin dan yield vanillin. Hasil penelitian untuk analisis optimasi menunjukkan bahwa faktor volume pelarut etil asetat dan lama waktu ekstraksi berpengaruh secara kuadratik terhadap respon kadar vanillin dan yield vanillin. Hasil solusi optimal diperoleh pada perlakuan dengan volume pelarut etil asetat sebesar 101,1 ml dan lama ekstraksi selama 123,5 menit. Hasil prediksi solusi optimal diperoleh kadar vanillin 0,014% dan yield vanillin 7,302 μg/g dengan ketepatan 92,8%. Validasi yang dilakukan berdasarkan pada prediksi solusi optimal diperoleh respon kadar vanillin 0,013% dan yield vanillin 6,950 μg/g. Hasil validasi kadar dan yield vanillin tersebut memiliki perbedaan masing-masing 4,081% dan 4,826% lebih rendah jika dibandingkan dengan prediksi pada solusi optimal. Kata kunci: etil asetat, kadar vanillin, yield vanillin
... The amount of material and the volume of solvent used also has a significant effect on the extraction results of vanillin compounds [54] as does the duration of the extraction process also affects the extraction results obtained [55]. Jadhav et al. [56], suggests that the longer the extraction the greater the vanillin yield obtained, but the vanillin yield decreases beyond the optimal point due to the solvent becoming saturated. The model of vanillin yield (Figure 4b) also shows the vanillin yield increases with increasing volume of ethyl acetate and extraction time. ...
... Further extraction beyond this time appears to have a marginal effect on the yield of vanillin. Research by Jadhav et al. [56], also showed that the ratio of the volume of solvents and materials had a significant effect on the yield of vanillin. The current work suggests that optimization of time and solvent used can be critical for achieving cost efficiencies. ...
... Ethyl acetate may extract nearly 35% more vanillin compared to the ethanol. The results of the optimal solution have prediction of vanillin levels obtained at 0.408% and vanillin yield of 3.957 μg g −1 with a [56], also showed that the ratio of the volume of solvents and materials had a significant effect on the yield of vanillin. The current work suggests that optimization of time and solvent used can be critical for achieving cost efficiencies. ...
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Value-added chemicals, including phenolic compounds, can be generated through lignocellulosic biomass conversion via either biological or chemical pretreatment. Currently vanillin is one of the most valuable of these products that has been shown to be extractable on an industrial scale. This study demonstrates the potential of using rice straw inoculated with Serpula lacrymans, which produced a mixture of high value bio-based compounds including vanillin. Key extraction conditions were identified to be the volume of solvent used and extraction time, which were optimized using response surface methodology (RSM). The vanillin compounds extracted from rice straw solid state fermentation (SSF) was confirmed through LC-ESI MS/MS in selective ion mode. The optimum concentration and yield differed depending on the solvent, which was predicted using 60 mL ethyl acetate for 160 min were 0.408% and 3.957 μg g−1 respectively. In comparison, when ethanol was used, the highest concentration and yields of vanillin were 0.165% and 2.596 μg g−1. These were achieved using 40 mL of solvent, and extraction time increased to 248 min. The results confirm that fungal conversion of rice straw to vanillin could consequently offer a cost-effect alternative to other modes of production.
... When choosing or optimising an extraction technique, it is critical to consider its efficiency and efficacy. The term efficiency refers to the yield of the extract, whereas efficacy refers to the potency of the extract (Jadhav et al., 2009). ...
... Among the experiments conducted, the RE technique and water were found to be the most appropriate technique and solvent, respectively. Furthermore, based on recent literature, many researchers have used the ultrasonic extraction technique to obtain a high yield of targeted compounds (Jadhav et al., 2009;Dong et al., 2010;Roselló-Soto et al., 2015). Ultrasonic extraction uses ultrasonic wave energy in the extraction. ...
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Coccinia grandis (L.) Voigt (family: Cucurbitaceae) is a popular leafy vegetable in Sri Lankan diet. C. grandis is high in phenolics and flavonoids. The present work attempted to determine a suitable extraction technique, and further optimise it to obtain phenolic-and flavonoid-rich extract from C. grandis leaves, with an aim at developing a nutraceutical targeting the dietary management of diabetes mellitus. Acetone extraction (AE), methanol extraction (ME), pre-warmed water extraction (PWE), electric shake extraction (ESE), reflux extraction (RE), ultrasonication with water (UEw), ultrasonication with ethanol (UEe), ultrasonic assisted-reflux extraction (URE), and reflux assisted-ultrasonic extraction (RUE) were chosen as the extraction techniques. URE was selected as a satisfactory extraction technique for further optimisation for the preparation of phenolic-and flavonoid-rich extract based on the contents of phenolics (32.97 ± 0.41 mg of equivalent gallic acid/g of extract) and flavonoids (4.50 ± 0.04 mg equivalent quercetin/g of extract). The highest yield of 32.8% was obtained by the URE technique. The optimal extraction conditions for URE were determined with an ultrasonic time of 19 min, refluxing time of 168 min, and liquid:solid ratio of 16.4 mL/g. This is the first attempt to investigate the selection and optimisation of an extraction technique for obtaining phenolic-and flavonoid-rich extract from C. grandis leaves. The present findings would be useful in the development of a commercially viable nutraceutical using a phenolic-and flavonoid-rich extract of C. grandis.
... En esta investigación se siguió el proceso de curado tradicional de los granos de V. planifolia según la antigua cultura totonaca. Después de recoger las vainas de V. planifolia, se sumergieron en agua caliente durante 5 a 8 segundos, un proceso conocido como muerte vegetativa [33]. Después, los cultivos se expusieron directamente a la luz solar durante una o dos horas hasta alcanzar 48 a 50 °C de temperatura superficial. ...
... Finalmente, de acuerdo con la concentración de vainillina en los tres cultivares evaluados, a pesar del bajo costo de producción de vaina de V. planifolia en los cultivares tradicionales, pero dependiendo de la concentración de vainillina se podría requerir más superficie de terreno para obtener un kg de vainillina. De Guzman y Zara (2012) sostienen que el rendimiento de la vainillina depende básicamente de las condiciones agroclimáticas, el sistema de cultivo, la polinización, la cosecha y el curado [33]. Por otro lado, Ramachandra y Ravishankar (2000) estimaron que, para producir 1 kg de vainillina son necesarios 500 kg de granos (basados en 2,0 g/Kg de vainillina); esto significa aproximadamente 40.000 flores polinizadas [34]. ...
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In this work we performed a characterisation of the production of Vanilla planifolia beans from tree communities of the Totonacapan region in Mexico and three cultivars' systems: traditional or coffee type, semitechnified or acahual and technician or mesh shadow. 95% of the traditional cultivars have been historically safely sheltered by the totonaca culture. From an economic point of view, the traditional cultivars are profitable, considering that vanilla beans are commercialized without a curing process. Knowledge of the aromatic profile of local vanilla beans allows cost improvement. In this research, the concentration of vanillin was analyzed, finding a considerable variation among cultivars, being necessary to consider differential pricing according to the location of the cultivars. Keyword-Cultivar type; deterministic model; economic analysis; market price; Vanilla planifolia; vanillin.
... Therefore, this analysis is highly important since the consumption of these fruits can provide many beneficial properties. It has been reported that the effect of various extraction parameters, such as type of the solvent, the number of beans, and the method of extraction (Soxhlet extraction and ultrasound-assisted extraction), influence the content of vanillin obtained from cured vanilla beans [50]. In this study, extraction was carried out with 70% methanol. ...
... Of the six underutilized fruits studied, Ugurassa showed the highest dietary fiber content. Barbados cherry showed the highest antioxidant efficacy, as measured by TPC, FRAP and IC 50 values. The underutilized fruits tested are rich sources of K, Ca, and P. Despite their richness in nutrients and antioxidant activity, these fruits remain underutilized in Sri Lanka. ...
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Sri Lanka has been identified as one of the world’s biodiversity hotspots with a rich array of fruits; however, most of them remain underutilized. The present study was carried out to investigate the nutritional composition and to assess the bioactivity of six underutilized fruits collected from three provinces of Sri Lanka. The selected fruit species were Màdan (Syzygium cumini), Maha Karamba (Carissa carandas), Himbutu (Salacia chinensis), Ugurassa (Flacourtia indica), Barbados cherry (Malpighia emarginata), and Ceylon gooseberry (Dovyalis hebecarpa). The proximate composition, total dietary fiber content, mineral content, total phenolic content, and vanillin contents were determined using standard methods. The antioxidant activity of methanolic extracts of fruits was assessed using FRAP and DPPH assays. Uguressa extract exhibited the highest dietary fiber content (12.25 ± 0.29 of fresh fruit weight) while the lowest was observed in Barbados cherry (6.01 ± 1.10 g/100 g). The total phenolic content (TPC) of fruits ranged from 6.8 ± 0.4 to 10.3 ± 0.3 milligram gallic acid equivalents/g fruit. Barbados cherry showed the highest antioxidant activity (AOA) as measured by FRAP (0.022 ± 0.003 mM Fe 2+/g fruit) and the highest vanillin content (2.4 mg/kg). The highest potassium (434.60 ± 0.36 mg/kg), phosphorous (16.69 ± 0.46), and calcium contents (23.43 ± 0.45) were observed in Uguressa. Màdan had the highest content of magnesium (13.25 ± 0.38 mg/kg), sodium (5.28 ± 0.30), iron (0.65 ± 0.12 mg/kg), and aluminum (1.15 ± 0.16 mg/kg). The highest manganese content (0.98 ± 0.18 mg/kg) was observed in Himbutu while the highest copper content was found in Uguressa (0.11 ± 0.04 mg/kg) and Maha Karamba (0.11 ± 0.03 mg/kg). The study reveals that six underutilized fruits tested possess high nutritional value and are rich in antioxidant activity.
... Ultrasound can be conveniently used to increase the rate of extraction through increased rate of mass transfer based on the turbulence and liquid streaming. Ultrasound effects can also cause rupture of cell wall and reduce the size of particle leading to greater yield of product through enhanced solvent penetration and the rates of diffusion [33,34]. In summary, the collapse of cavitation bubbles develops high-speed liquid circulation currents, micro-turbulence, a perturbation in micro-porous particles and inter-particle collisions of the plant material which leads to enhancement in internal diffusion and eddy diffusion rates [33,35]. ...
... Ultrasound effects can also cause rupture of cell wall and reduce the size of particle leading to greater yield of product through enhanced solvent penetration and the rates of diffusion [33,34]. In summary, the collapse of cavitation bubbles develops high-speed liquid circulation currents, micro-turbulence, a perturbation in micro-porous particles and inter-particle collisions of the plant material which leads to enhancement in internal diffusion and eddy diffusion rates [33,35]. Furthermore, cavitation also results in an infringement over the surface due to micro-jets with consequent erosion and surface peeling [36]. ...
Article
The present study deals with intensified extraction of curcumin from Curcuma aromatica by employing ultrasound-assisted extraction (UAE) approach also elucidating comparison with the conventional batch extraction to highlight the intensification benefits based on the usage of ultrasound. Understanding into the effect of operational parameters like type of solvent, extraction temperature, solid to solvent ratio and raw material size distribution as well as the equipment operating conditions as frequency and power on the extraction yield has been developed. Based on the results for extraction yield, the optimum conditions for UAE approach were 40 °C as temperature, 1:30 as solid to solvent ratio, 0.09 mm as the mean particle size, 240 W as ultrasonic power, 22 kHz as ultrasonic frequency and ethanol as the most suitable solvent. Under these optimum conditions, the highest extraction yield of 73.18 % was achieved in 2 h whereas batch extraction for 14 h resulted in 52.31 % yield clearly demonstrating the intensification due to ultrasound. Peleg's model was applied to explain the extraction kinetics of curcumin and the proposed model satisfactorily predicted the extraction kinetics of curcumin. Overall, UAE proved to be a better technique in terms of lesser time, lesser heating requirement and additional extraction yield.
... To the best of our knowledge, the application of M and U technologies during the CP have not been studied. These technologies have been used primarily for the extraction of vanillin from cured vanilla beans with encouraging results [12,13]. About this, Dong's research [14] compared ultrasoundassisted extraction, pressure-assisted extraction, and microwave-assisted extraction of vanillin from Vanilla planifolia, where microwave-assisted extraction showed the strongest extraction power, shortest time, and highest antioxidant activity. ...
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The curing process (CP) of Vanilla planifolia pods, which is a long and tedious process, is necessary to obtain the natural vanilla extract. This research evaluated the application of microwave (M) and ultrasound (U) during the “killing” stage of the CP and its effect on vanillin content and β-glucosidase activity. The pods were immersed in a container with water or with moistened samples for the M treatments. In U treatments, the pods were immersed in an ultrasonic bath. After this stage, the samples were subjected to an additional U treatment. The results show that the application of these technologies significantly improves vanillin yield (p < 0.05) and the curing time is reduced to 20 days. U treatments subjected to additional sonication at 38 °C obtain more than double the yield of vanillin regarding control. The effect of M and U on cell structure damage increases with additional sonication, but at 15 min, β-glucosidase inactivation decreases the final yield. Disposition of samples in M also affects the final vanillin content. There is no significant correlation between β-glucosidase and vanillin in the different treatments. The application of M and U with the appropriate parameters reduces the CP time without affecting the compounds of interest.
... Mechanical effects are attributed to shear stress, turbulence and collapse pressure (Lateef et al., 2007) whereas, chemical effect includes sonolytic effects owing to formation of free radicals (Hu et al., 2006). Lower operating temperatures played pivotal role in application of ultrasonication for extraction of compounds from biological matrices (Jadhav et al., 2009). Ultrasonication has been used for extraction of grapeseed oil (Da Porto et al., 2013), soybean oil (Li et al., 2004) and reported increased amount of polyphenol from grape seed oil and improved saturated fatty acid from soybean oil compared with conventional extraction. ...
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Ghee is a major Indian dairy product with a pleasant flavor. During its manufacture, ghee residue is obtained as the by‐product, which consists of substantial quantity of phospholipids. Phospholipids exhibit emulsifying properties and offer some health benefits. The present study aimed to optimize the process parameters for the extraction of phospholipids from ghee residue (GR) using ultrasonication. The GR was subjected to a series of pre‐treatments before ultrasonication. The hot water treatment led to reduction in nonpolar lipids and improved polar lipids (35.47% fat basis). Taguchi orthogonal array design was employed for optimization of ultrasound power, treatment temperature, time and solvent:solid (S:S) ratio with phospholipid content and antioxidant activity as the response variables. The phospholipid content ranged between 18.54% and 23.89% and antioxidant activity of the extracted samples varied from 47.01% to 50.64% expressed as radical scavenging activity by DPPH assay, while for the untreated GR, the PL and antioxidant activity were 4.98% and 32.75%, respectively. The power level of 80%, 80°C treatment temperature, S:S ratio of 15 and sonication time of 4 min. resulted in maximum extraction of phospholipids (24.12%). The yield of phospholipids was quantified as 13.1% and 8.88% by two elution techniques using solid phase extraction methods. The predicted and experimental values for the responses were in good agreement with R² value of 0.98. Power and temperature were found to be significant (p < 0.01) in influencing phospholipids yield. For antioxidant activity of the extract, S:S ratio exerted significant effect (p < 0.01). The experimental data were fit in four defined empirical models for understanding the extraction kinetics. Based on the R² values, the models explained the kinetics in the following order: Parabolic model>Power law>Peleg's model>Elovich's model. Practical applications Presently, ghee residue is often discarded as waste or used as animal feed by most of the ghee manufacturing dairy plants. Few studies were conducted to incorporate ghee residue as an ingredient in different food products. However, the present study opens new avenues for utilization of this by‐product for extraction of high value bioactive components, that is, phospholipids, with the help of novel technology; namely ultrasonication. The phospholipids have techno‐functional properties as an emulsifier. One of the classes of phospholipids, that is, sphingomyelin has unique health benefits, therefore this extract will also have scope as a nutraceutical. Thus, there is great practical utility for the present findings. In addition, for the scaling up of extraction techniques, the understanding of mass transfer kinetics is very vital and the same had been studied in the present investigation. Thus, the findings of this study are helpful in determining the ideal ultrasound‐assisted extraction conditions for extraction of phospholipids from ghee residue. Kinetics of extraction will help to explore opportunities for scale‐up of the process.
... Les méthodes d'extractions conventionnelles (ou classiques) sont basées sur une opération de séparation solide -liquide : un objet solide est mis en contact avec un fluide liquide (ou gazeux). Les composants d'intérêt du solide sont transférés par solubilisation dans le fluide.Les méthodes d'extractions conventionnelles ont plusieurs inconvénients tels que : les résistances de transfert de masse dans des milieux hétérogènes[239] ou les difficultés rencontrées lors de l'élimination du fluide qui risque d'entraîner la perte de composés volatils[240].Cependant, malgré ces inconvénients, les techniques d'extraction conventionnelles demeurent des procédures d'extraction couramment utilisées. Pendant de nombreuses années, les techniques conventionnelles ont été largement acceptées, principalement en raison de leur facilité d'utilisation, de leur efficacité et de leur applicabilité étendue [241]. ...
Thesis
Cette étude se déroule en deux parties, la première partie est consacrée à la mise en place d’une méthodologie dans le but d’isoler les métabolites secondaires. La seconde partie décrit les propriétés phytochimiques de poudres issues de matrices végétales en fonction de leur granulométrie. Dans la première partie, qui est consacrée à l’isolement de métabolites secondaires par HPLC semi-préparative, la mise en place du processus d’isolement de l’hédéracoside C et l’α-hédérine, a été effectuée à partir d’extraits de parties aériennes du lierre (Hedera helix L.). La généralisation de ce processus d’isolement appliqué aux extraits de parties aériennes du millepertuis (Hypericum perforatum L.) a permis d’isoler avec succès un hypéroside qui est un des flavonoïdes marqueur du millepertuis. Le but de cette deuxième partie est dans un premier temps, de valider le procédé de broyage et de tamisage du matériel végétal : PTC « Pulvérisation & Tamisage différentiel Contrôlés » à l’échelle industrielle pour la production de différentes classes granulométriques des poudres. A cet effet, les résultats d’analyses phytochimiques de classes granulométriques de neuf plantes de la Région Lorraine obtenues par PTC à l'aide d’un pilote industriel sont comparés à ceux obtenus à l’échelle du laboratoire. Les plantes sélectionnées snot : le fenouil (Foeniculum vulgare Mill.), le saule blanc (Salix alba L.), le millepertuis (Hypericum perforatum L.), l’ortie (Urtica dioica L.), la solidage (Solidago virgaurea L.), la piloselle (Hieracium pilosella Vaill.), le rosier des chiens (Rosa canina L.), la griffe du diable (Harpagophytum DC.) et le lierre (Hedera helix L.). L’évaluation de l’activité antioxydante ainsi que les analyses effectuées par LC-MS indiquent que la production des poudres à l’échelle du laboratoire est généralisable à l’échelle industrielle.Par ailleurs, pour la première fois, l’application à quatre fruits : la cerise (Prunus avium L.), la pêche (Prunus persica L.), la quetsche (Prunus domestica subsp. Insititia L.) et la mirabelle (Prunus domestica subsp. Syriaca) de la Région Lorraine du procédé PTC à l’échelle du laboratoire montre que l’extraction par voie sèche est une nouvelle méthode pour enrichir certaines classes granulométriques en composés bioactifs.
... Soxhlet, hydro-distillation and alcohol maceration are some of the current methods for extracting essential oils, fats, and oils from plant tissues (Wang and Weller, 2006). Traditional Soxhlet extraction methods are frequently rendered ineffective due to high mass transfer resistances caused by the system's multi-phase composition (Jadhav et al. 2009). Depending on the diffusion speeds of the solvents, this separation procedure might take a long time to achieve results. ...
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An astonishing number of essential nutrients and phytochemicals may be found in the by-products of the apple juice business. This comprehensive study found that apple wastes and by-products may be employed as fortifying elements in plant food items, meat and dairy products, as well as in other food products. The high dietary fiber content of apple waste and by-products were translated to the treated end-product, enhancing its nutritional value. Due to apple waste and by-products, which are the primary polyphenolic source of the entire fruit, an increase in the antioxidant activity has been reported. In plants, fortification led to an undesired shift in hue to a reddish one, although this change was well received in processed meat by the sensory panel.
... Em geral, as frequências variam entre 20 e 100 MHz(Xu et al., 2021). Basicamente, o principal fenômeno produzido pelo ultrassom é a cavitação acústica, que é conhecida por gerar diversos efeitos na matriz vegetal, como a circulação do líquido (agitação do solvente utilizado) no sistema e a geração de turbulência que pode auxiliar no aumento da transferência de massa(Jadhav et al., 2009). Dessa forma, a extração assistida por ultrassom requer uma energia adicional de ultrassom para criar bolhas de cavitação que produzem efeitos mecânicos e térmicos nas células vegetais. ...
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Devido a projeção de crescimento populacional para as próximas décadas, a demanda pela produção de alimentos vem desencadeando um aumento na geração de subprodutos agroindustriais. No passado, esses subprodutos eram vistos como uma problemática a ser solucionada, porém, no cenário atual, eles podem servir como matéria-prima para diversas indústrias, sendo a principal estratégia utilizada para o desenvolvimento de produtos e processos e, também, para a extração de compostos de interesse, como os compostos bioativos. Os compostos bioativos são divididos em grupos contendo várias substâncias e, dentre elas, destacam-se os polifenóis e carotenoides, que podem expressar atividades biológicas e funcionais importantes, despertando a atenção para sua extração. Neste contexto, a aplicação de tecnologias inovadoras de extração nas indústrias de alimentos tem sido amplamente estudada e investigada, principalmente devido ao aumento da consciência dos consumidores por opções mais ecológicas que não incluam a utilização de solventes orgânicos nocivos à saúde. Dessa forma, extrações assistidas por tecnologias não convencionais ou emergentes como ultrassom (US), micro-ondas (MO), fluído supercrítico (FS), fluído pressurizado (FP), alta pressão hidrostática (AP) e campo elétrico pulsado (CEP) têm demonstrado diversas vantagens quando comparadas aos métodos de extração tradicionais, como uso de temperaturas moderadas e menor tempo de extração, porém ainda enfrentam barreiras para sua inserção à nível industrial. Portanto, esta revisão visa apresentar os compostos bioativos provenientes de frutas e vegetais e seus métodos de extração, enfatizando o potencial das tecnologias emergentes para tal finalidade.
... This method has been widespread for plant oil extraction [42] and some organics such as vanillin [43], coffee [44], marijuana cigarette [45], and orange juice [46]. In this method, the substance is constantly exposed to a stream of the solvent during the operation. ...
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... In recent studies, UAE was proven as a save energy method [101] which could create massive effects in a very short time [16]. UAE improved the extraction efficiency by two mechanisms: (a) the penetration of solvent across the tissue and (b) rinsing the component inside the plant cell after weakening the cell wall [103,104]. Mason [105] reported that ultrasound waves generate intense shear force, microturbulences, and shock waves. During the treatment, extreme motion energy transforms to heat, which induces mass transfer [84,101]. ...
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In recent years, the improvement of curcumin recovery from turmeric by cell and tissue disintegration techniques has been gaining more attention; these emerging techniques were used for a reproducible and robust curcumin extraction process. Additionally, understanding the material characteristics is also needed to choose the optimized technique and appropriate processing parameters. In this review, an outlook about the distribution of different fractions in turmeric rhizomes is reviewed to explain matrix challenges on curcumin extraction. Moreover, the most important part, this review provides a comprehensive summary of the latest studies on ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), enzyme-assisted extraction (EAE), high-pressure-assisted extraction (HPAE), pulsed electric field-assisted extraction (PEFAE), and ohmic heating-assisted extraction (OHAE). Lastly, a detailed discussion about the advantages and disadvantages of emerging techniques will provide an all-inclusive understanding of the food industry’s potential of different available processes.
... This indicated that the pre-leaching step could increase CY and DPPH by improving cell wall permeability, and by increasing the swelling of the plant sample, thus providing a larger surface area for the ultrasound waves to affect sample cell walls (Chemat et al., 2017). This has been supported by Jadhav et al. (2009) who found that a pre-leaching of 30 min improved the yield of vanillin extracts from vanilla pods after 60 min of UAE. Poodi et al. (2018) reported a similar observation on the crude yield extracts from Feijoa leaves; 40 min of pre-leaching significantly increased the yield of extracts. ...
Article
The present work demonstrated the bioactive compound recovery from Bentong ginger (Zingiber officinale Roscoe var. Bentong) using ultrasound-assisted extraction (UAE) in terms of crude yield (CY), as well as total phenolic content (TPC), 1,1-diphenyl-2-picrylhydrazyl (DPPH), and ferric reducing-antioxidant power (FRAP), which reflected the antioxidant properties. These response variables were evaluated as functions of the independent variables; temperature (30 - 60°C), time (10 - 30 min), and ultrasonic intensity (1768 - 5304.10 W/cm2), using response surface methodology (RSM). The variables were optimised using quadratic polynomial through the correlations calculated from the regression models fitted to the experimental data. The predicted values of CY, TPC, FRAP, and DPPH under the optimal conditions (40°C, 3536.78 W/cm2, and 25 min) were 23.42%, 778.08 mg GAE/g, 636.08 µmol Fe2+/g, and 150.01%, respectively. These experimental values were well fitted with the predicted values, except for DPPH. With UAE set at the optimal conditions, a pre-leaching step (PLS) was added to the process to investigate its effect on the extraction. It was found that PLS-UAE produced higher extraction yields (30.15%); however, the antioxidant activity of the extracts was significantly (p < 0.05) higher at the optimised condition for UAE only treatment. The PLS application led to structural cell damage which increased CY, and this was validated through scanning electron microscopy (SEM).
... The time given for the extraction, solvent, and the frequency are the important parameters. The time taken for the extraction of saponins and related compounds is relatively less when compared to conventional methods like soxhlet extraction (Jadhav et al. 2009). Microwave-assisted extraction is most accepted technique for the isolation of metabolites in the recent times (Deore et al. 2015). ...
Chapter
Plants have been utilized as food, feed, and fodder since the dawn of civilization. Plants are also thought to be a rich source of bioactive compounds with a variety of pharmacological actions. Saponins are one such group of molecules which are present in various plant species. As triterpenoid glycosides, they have a 30C oxidosqualene precursor aglycone moiety (sapogenin), which is then linked with glycosyl residues to form saponin. These saponins have a unique platform in the field of pharmaceutical and nutraceutical industries. Saponins are used for the treatment of various diseases which include cancer, diabetic, cardiac, hepatic, and nervous disorders. The production of saponins through conventional approaches is time-consuming and hard to extract pure compounds, and thus to achieve this, in vitro methods have been developed and enhanced the production and extraction of the metabolites. The present chapter focuses on the in vitro production of saponins through various tissue culture techniques such as shoot, callus, cell suspension, adventitious root, hairy root culture, and applications of bioreactors at commercial level. The chapter also focuses on biosynthetic pathway, extraction methods, and biological activities of saponins.KeywordsSaponinsPlant secondary metaboliteIn vitro productionBiosynthesisPharmacology
... Polarity of solvents has a significant impact on the extraction efficacy since the solubility range of the natural components increases with increasing order of polarity. [18,19] Thus, the results reveal that high polar solvent attributes high dissolution of active compound present in P. schmidtii fruit might be contributed to the phenolic compounds in the extracts which have high effectiveness as antioxidants. [20,21] ...
Article
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Aim: The present study aims at screening the phytochemical components and evaluates the antioxidant, anti-bacterial, and anti-inflammatory activity of fruit of Piper schmidtii, an endemic plant species from The Nilgiris, Tamil Nadu. Materials and Method: The different polar solvents such as petroleum ether, chloroform, ethyl acetate, methanol, and water were used and extraction was carried out using the soxhlet apparatus. The extracts were screened for qualitative and quantitative phytochemical analysis. The extracts of P. schmidtii were also subjected to in vitro-antioxidant activity by DPPH assay, Phosphomolybdenum assay, Ferric reducing antioxidant power (FRAP), superoxide radical scavenging activity, and reducing power assay. Results: Among all the extracts, methanol extract exhibited the maximum amount of phenolics (731.91 mg GAE/g extract), tannin (726.6 milligrams of Gallic acid equivalent/g extract), and ethyl acetate extract depicted the maximum quantity of flavonoids (698.17 mg QE/g extract). Methanol extract of P. schmidtii revealed the higher antioxidant activity in all the assays with IC50 values of 15.19 μg/ml (DPPH), 135.67 mg AAE/g (Phosphomolybdenum assay), 380.98 mM Fe/mg (FRAP), 60.94% (Superoxide) and higher reducing power was depicted in the ethyl acetate extract, respectively. Further anti-bacterial activity revealed that the methanol extract shows highest inhibitory activity against the tested bacterial pathogens. The methanol extract showed high degree of inhibition (71.24%) in anti-inflammatory assay. Conclusion: Thus, the result support that P. schmidtii is a potential source of natural antioxidant that can inhibit bacterial growth and subside inflammation.
... In general, the extracting solvent is heated to boiling and the condensed solvent vapors are passed through a cellulose or glass thimble containing the material to be extracted. The filtrate runs back into the reservoir of boiling solvent completing the cycle (Jadhav et al., 2009;Sagar et al., 2018). ...
Article
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Truffles are considered one of the world's most highly prized foods mainly due to their desirable organoleptic properties and rarity. However, truffles are seasonal (harvested mostly in winter from June to August in the Southern Hemisphere and from December to February in the Northern Hemisphere) and extremely perishable. Truffles deteriorate rapidly showing undesirable changes within 10 days from harvest in aroma and visual appearance after harvest. The very short postharvest shelf life (about 7–10 days) limits the potential for export and domestic consumption all year round. Several preservation methods have been studied to prolong their shelf life without the loss of aroma. However, all traditional preservation techniques have their own shortcomings and remain challenging. The extraction of natural truffle aroma volatiles for food applications could be a potential alternative to replace the existing synthetic flavoring used for processed truffle products. Four commonly used extraction methods for recovering volatile compounds from plants, namely, supercritical carbon dioxide extraction, Soxhlet extraction, distillation, and cold pressing, are critically analyzed. Up to date, existing research about the extraction of aroma volatiles from truffles is limited in the literature but based on the volatility of the key truffle volatile compounds, supercritical carbon dioxide extraction may offer the best possibility so that a natural truffle‐based product that can be used in food applications throughout the year can be made available.
... For example, when Shakeel et al. (44) evaluated the solubility of vanillin in ten different environmentally green solvents, they observed a relatively high mole fraction solubility of vanillin (T = 298-318 • K) in ethanol (7.94 × 10 −2 at 298 • K) and propylene glycol (7.15 × 10 −2 at 298 • K), which was significantly higher than water (1.23 × 10 −3 at 298 K) at each temperature investigated. Similarly, in another work (45), it was observed that extraction of vanillin was higher in polar solvents such as ethanol and methanol and least in the case of non-polar solvent such as hexane, suggesting ethanol as an optimum solvent for maximum yield of vanillin. ...
Article
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In this work, the effect of pulsed electric field (PEF) pre-treatment on the extractability in green solvents (i. e., ethanol–water mixture and propylene glycol) of target aroma and bioactive compounds, such as vanillin from vanilla pods, theobromine and caffeine from cocoa bean shells, linalool from vermouth mixture, and limonene from orange peels, was investigated. The effectiveness of PEF as a cell disintegration technique in a wide range of field strength (1–5 kV/cm) and energy input (1–40 kJ/kg) was confirmed using impedance measurements, and results were used to define the optimal PEF conditions for the pre-treatment of each plant tissue before the subsequent solid–liquid extraction process. The extracted compounds from untreated and PEF-treated samples were analyzed via GC-MS and HPLC-PDA analysis. Results revealed that the maximum cell disintegration index was detected for cocoa bean shells and vanilla pods ( Z p = 0.82), followed by vermouth mixture ( Z p = 0.77), and orange peels ( Z p = 0.55). As a result, PEF pre-treatment significantly enhanced the extraction yield of the target compounds in both solvents, but especially in ethanolic extracts of vanillin (+14%), theobromine (+25%), caffeine (+34%), linalool (+114%), and limonene (+33%), as compared with untreated samples. Moreover, GC-MS and HPLC-PDA analyses revealed no evidence of degradation of individual compounds due to PEF application. The results obtained in this work suggest that the application of PEF treatment before solid–liquid extraction with green solvents could represent a sustainable approach for the recovery of clean labels and natural compounds from aromatic plants and food by-products.
... The ultrasonication treatment using methanol 80% (v/v) resulted in a slightly higher phenol content 21.88 ± 0.34 mg/g in comparison to conventional extraction method. Jadhav et al. [18], while extracting vanillin from vanilla pods, reported an increase of almost 20% of vanillin by ultrasonication than the conventional solvent extraction. The lowest value of phenolic compounds from refluxing is due to the thermal degradation of the polyphenols due to higher temperature [19]. ...
Article
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The present study was conducted to study the different extraction methods, i.e., refluxing, ultrasonication (US), and supercritical fluid extraction (SFE), for their efficacy in extracting the phytochemicals from kinnow peel, grown in Punjab India. The aqueous solvent resulted in higher extraction of phenols and flavonoids by 0.5–1% in comparison to absolute solvents. Also, in all extraction techniques, 80% methanol increased the phytochemical extraction by 1–2%. However, comparing the different extraction methods, results revealed that the extracts obtained after SFE exhibited highest total phenols (27.91 ± 0.05 mg GAE/g) and total flavonoids content (10.31 ± 0.39 mg/g). The extraction of other phytochemicals viz carotenoids, β-carotene, and ascorbic acid was also highest with SFE method. While the degree of extraction varied with ethanol being highest for ascorbic acid and acetone for carotenoids and β-carotene. Furthermore, the characterization of phytochemical extracts by liquid chromatography–mass spectrophotometry identified phloretic acid, p-coumaric acid, dicaffeoylquinicacid, hesperetin 7-O-methyl ester, cinnamic acid, 5-O-feruloylquinic acid, 3-p-coumaroylquinic acid, diosmetin, quercetin, kaempferol, trihydroxydimethoxyflavone, narirutin, and β-carotene, as major bioactive compounds. Fourier transform infrared spectroscopy and scanning electron microscopy revealed that SFE-CO2 resulted in prominent channeling effect explaining the highest extraction efficiencies of the method. The extracts from kinnow peel can therefore be utilized as functional ingredients in various foods and pharmaceuticals.
... Numerous chemical and mechanical processes like solvent extraction and steam distillation are used for the extraction of compounds from plants (Shirsath et al., 2012). The existing techniques used for the extraction of essential oils, fat and oils include Soxhlet extractor, hydrodistillation and maceration with alcohol (Jadhav et al., 2009). The mass transfer resistance due to the involvement of more than one phase within the system repeatedly limits the use of the traditional Soxhlet extractor technique (Danlami et al., 2014). ...
Article
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Purpose The purpose of this study was to evaluate the extract of Moringa stenopetala seed oil, by organic solvents (methanol and hexane), for its efficacy against microbial activity on cotton fabrics. The selected microbes for the study were two types of bacteria which are Gram-positive (S. aureus) and Gram-negative (E. coli). Design/methodology/approach Two types of bacteria, Gram-positive (S. aureus) and Gram-negative (E. coli) were used. The extract was applied on fabrics at a concentration of 5, 10 and 15 g/L using the pad-dry-cure method and antibacterial activities verified by the bacterial-growth reduction method. The treated fabrics were evaluated for antimicrobial activity against the bacteria before and after 15 washing cycles. The extract was examined for molecular structural change using fourier transform infrared spectroscopy (FTIR) and physical properties of the fabric; tensile strength, elongation, air permeability, stiffness and wettability were evaluated. Findings Results showed treated fabrics reduces the growth of Gram-positive (S. aureus) and Gram-negative (E. coli) bacteria from 77.6%–100% before wash and 45.8%–85.2% after wash for both extract concentrations. Comparing extracts, hexane extract reduces all bacteria growth than methanol extract for both extract concentrations while S. aureus was more susceptible to antimicrobial agents than E. coli at a lower concentration. As result, the tensile strength and air permeability were relatively lower than untreated ones without affecting the comfort properties of the fabric. Originality/value This study indicates that the Moringa stenopetala seed oil extract has a strong antimicrobial activity.
... Perusahaan terkenal prancis memperoduksi vanilin melalui senyawa asam ferulik dengan harga kisaran USD 700/kg, harga bisa mencapai kisaran USD 1.800/kg jika vanilin berasal dari biji vanila, sedangkan untuk sintesis vanilin seharga USD 15/kg (Martău et al., 2021). Saat ini, vanilin sudah diproduksi dalam skala industri dengan jumLah 20.000 ton per tahun dan 15% bahan baku yang digunakan berasal dari lignin (3.000 ton/tahun) (Holladay et al., 2007;Jadhav et al., 2009). Ekstraksi vanilin dengan pelarut organik etil asetat dianggap sangat baik, untuk mengekstrak senyawa vanilin dikarenakan senyawa semi polarnya yang dapat mengikat senyawa spesifik aromatik termasuk vanilin dari komponen fenolik (Popescu et al., 2020) Oleh (Nurika et al., 2020). ...
Article
Limbah tandan kosong kelapa sawit (TKKS) merupakan limbah hasil produksi minyak sawit yang memiliki kandungan lignoselulosa (lignin, selulosa, hemiselulosa) tinggi, dapat dimanfaatkan untuk produksi senyawa aromatik vanilin dengan menggunakan jamur Phanerochaete chrysosporium dan pelarut etil asetat. Diketahui pelarut etil asetat dan lama ekstraksi berpengaruh terhadap kadar vanilin dan yield vanilin dengan Response Surface Methode (RSM) terdiri dari 4 faktor yang digunakan untuk mengukur sejauh mana faktor-faktor tersebut saling berpengaruh terhadap kadar vanilin. Regresi terdiri dari 13 titik faktorial dengan 6 titik aksial, dan 7 titik tengah melalui softwere Design Expert 7.0.0. Faktor-faktor optimasi digabung untuk mendapatkan nilai optimum untuk menghasilkan kadar dan yield vanilin yang bagus. Hasil penelitian optimasi RSM volume pelarut etil asetat yaitu 100,36 mL dan lama ekstraksi yaitu 120,27 menit yang digunakan dalam penelitian TKKS dengan nilai validasi optimal yang didapatkan yaitu kadar vanilin mendekati hasil prediksi sebesar 0,015% dan yield vanilin sebesar 11,862 µg/g. Hasil dalam penelitian ini menunjukkan penggunaan bio-pretreatment Phanaerocaete chrysosporium sebagai biokonversi TKKS menghasilkan vanilin dapat menekan biaya besar dan meningkatkan nilai fungsi dari limbah TKKS
... All four are widely distributed in several aromatic plants and its products. Carvacrol and thymol are primary components of thyme and oregano oils; eugenol is the main active compound of the oil extracted from clove and is also found in other plant sources such as basil, cinnamon or pepper; and vanillin is the main constituent of vanilla beans (Jadhav et al., 2009;Kachur and Suntres, 2020;Khalil et al., 2017). They are common flavouring agents in fragrances, cosmetics and food products, and are also used for other purposes in various industries like pharmaceutical, dentistry or agriculture (Kachur and Suntres, 2020;Memar et al., 2017;Nejad et al., 2017;Priefert et al., 2001). ...
Article
The extensive use of essential oil components in an increasing number of applications can substantially enhance exposure to these compounds, which leads to potential health and environmental hazards. This work aimed to evaluate the toxicity of four widely used essential oil components (carvacrol, eugenol, thymol, vanillin) using the in vivo model Caenorhabditis elegans. For this purpose, the LC50 value of acute exposure to these components was first established; then the effect of sublethal concentrations on nematodes’ locomotion behaviour, reproduction, heat and oxidative stress resistance and chemotaxis was evaluated. The results showed that all the components had a concentration-dependent effect on nematode survival at moderate to high concentrations. Carvacrol and thymol were the two most toxic compounds, while vanillin had the mildest toxicological effect. Reproduction resulted in a more sensitive endpoint than lethality to evaluate toxicity. Only pre-exposure to carvacrol and eugenol at the highest tested sublethal concentrations conferred worms oxidative stress resistance. However, at these and lower concentrations, both components induced reproductive toxicity. Our results evidence that these compounds can be toxic at lower doses than those required for their biological action. These findings highlight the need for a specific toxicological assessment of every EOC application.
... The beneficial effects of sound waves on extraction are attributed to the formation and asymmetrical collapse of micro cavities in the vicinity of cell walls leading to the generation of micro jets rupturing the cells (Mason et al., 1996). UAE provides better extraction of the vanillin in shorter time period for different solvents as compared to the Soxhlet method (Jadhav et al., 2009). ...
Chapter
A scientific definition of the term volatile oils is not possible, although several practical definitions exist. The most frequently used definition describe a volatile or an essential oil as a more or less volatile material isolated from an odorous plant of a single botanical species by a physical process. They are usually liquids which will evaporate or volatize when exposed to ordinary temperature and so they are called ethereal oils. A few of them are solid or resinous, and showing different colors ranging from pale yellow to emerald green and from blue to dark brownish red. These volatile oils are also called essential oils (EOs) because they were believed to represent the quintessence of odor and flavor from the flower kingdom – differ in composition properties from fatty or fixed oils, which consist for the most part of glycerides and from mineral or hydrocarbon oils. They are synthesized by all plant organs, i.e., buds, flowers, leaves, stems, twigs, seeds, fruits, roots, wood or bark, and are stored in secretory cells, cavities, canals, epidermic cells or glandular trichomes. There are several extraction methods for volatile oils extraction, comprising steam distillation, hydrodistillation, organic solvent extraction, expression, enfleurage, microwave-assisted distillation, microwave hydrodiffusion and gravity, high-pressure solvent extraction, supercritical carbon dioxide extraction, ultrasonic extraction, solvent-free microwave extraction, and the phytonic process. Volatile oils are mainly comprises of biosynthetically related groups which includes terpenes and their oxygenated derivatives such as aldehydes, ketones, alcohols, phenols, acids, ethers and esters having low molecular weight. Monoterpenes and sesquiterpenes are usually the main group of compounds found in essential oils. Moreover, some essential oils may also contain phenylpropanoids, fatty acids and their esters and, more rarely, nitrogen and sulfur derivatives. These oils find applications mainly in the flavor and fragrance industry, pharmaceutical industries. In recent years field of aromatherapy is evolved, which is the science of applying the controlled use of naturally plant extracted essences to promote physical and psychological well-being. The knowledge of these oils has been constantly developed and updated in the long stream of history thanks to a growing number of studies in multidisciplinary fields. Although some compositions and mechanisms are not completely understood, the fascinating odor of EOs and their interesting biological activities are of great interest, which have been pushing the progress of the EOs’ research in recent years. This chapter documents the conventional as well as novel extraction techniques for volatile oils with their specification in terms of their principles, benefits and disadvantages. The chapter also comprehensively reviews the chemistry of volatile oils and discusses their synthetic route.
... The collapsing cavitation bubbles are capable of destroying the EO glands and therefore promoting its release into the surrounding environment. Thus, ultrasound has been used for certain flavor extractions [20][21][22][23][24]. This extraction method provides both better yield, better quality of the extract and a gain in extraction time. ...
Article
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Knowing that flavored products would increase the use of olive oil by non-traditional consumers and enhance the added value of this valuable agricultural product, the virgin olive oil (VOO) was flavored with the seeds of Pimpinella anisum (Green anise) using three different methods: classic maceration, ultrasonic assisted maceration and direct addition of the essential oil (EO). These methods were compared under two main criteria: time and level of aromatization. The physico-chemical parameters and the thermal stability of flavored oils prepared by the three methods were determined by AOAC titration method and GC–MS analysis so as to compare the aromatization effect of the three methods. The trans-anethol is the major component of the EO of anise seeds as well as the indicator of the level of aromatization. GC/MS analysis results of the flavored oils showed that the diffusion of trans-anethol in the flavored oil by direct addition of EO was very important (36.3% of the total volatile fraction of the flavored oil) in comparison to the oil flavored by ultrasonic assisted maceration or classic maceration (respectively 26.59% and 23.85%). These different aromatization methods ensure an improvement in the quality of VOO with an enrichment in polyphenols estimated at 35% in the case of ultrasonic flavored oil, an increase in the content of carotenoids and chlorophylls (67% and 21% respectively) in the event of aromatization by classic maceration and a decrease in specific absorbency at 232 nm estimated at 29% during aromatization by addition of EO as well as a decrease in the peroxide value estimated at 26% in oil flavored by classic maceration unlike in oil flavored by ultrasound which has seen an increase of around 20%. The aromatization was able to maintain the stability of the oils and its qualification as VOO with a gain in induction time in the case of treatment at 60 °C estimated at 29 and 27.5 days respectively in oils flavored by addition of EO and by conventional maceration, an improvement resistance to degradation concerning K232 and K270 of all flavored oils which varied from 15 to 40 days in the case of treatment at 60 °C and 3 h resistance to degradation of oils treated at 130 °C for K232. Polyphenols, chlorophyll pigments and carotenoids play an important role in oxidative stability due to their antioxidant nature and their degradation during heating is very complex. All of these physico-chemical changes have increased the thermal stability of flavored oils with better resistance to oxidation of flavored oil by classic maceration in compared to oil flavored by adding EO and the oil flavored by using ultrasound.
... Several esters of eugenol (1) showed cytotoxicity against human breast cancer cells MCF-7 [6][7]. Oxidation of eugenol (1) has been reported to yield vanillin (2) which is widely used as flavor (in dairy products, chocolates, cakes, cola-type drinks), cosmetics, perfumes, pharmaceuticals, and food preservative [8][9][10][11][12][13][14]. Various vanillin (2) derivatives have been reported as fragrances/flavors [3,[15][16][17][18], and have antimicrobial activity [19]. ...
Conference Paper
Indonesia has the world’s largest Syzygium aromaticum plant area. Leaves and buds of this plant are distilled to yield clove essential oil. Separation of eugenol from clove oil and its transformation to various derivatives have been carried to increase added value of these oil. This paper reports transformation of eugenol to vanillin, vanillyl alcohol, and three new fragrances.
... Soxhlet extraction is an old yet effective method for plant oil extraction [48]. It has been used to extract organics from over a hundred types of biomass, including Sunn hempseeds [49], marijuana cigarette [50], hashish [51], coffee [52], vanillin [53], rice bran [54], walnut kernel [55], fungal biomass [56], algal oil [57,58], orange juice [59], etc. It operates based on a continuous cycle of solvent and leaving the extracts in the extract chamber and contacting the biomass in the batch process. ...
Article
Full-text available
Cannabis plant has long been execrated by law in different nations due to the psychoactive properties of only a few cannabinoids. Recent scientific advances coupled with growing public awareness of cannabinoids as a medical commodity drove legislation change and brought about a historic transition where the demand rose over ten-fold in less than five years. On the other hand, the technology required for cannabis processing and the extraction of the most valuable chemical compounds from the cannabis flower remains the bottleneck of processing technology. This paper sheds light on the downstream processing steps and principles involved in producing cannabinoids from Cannabis sativa L. (Hemp) biomass. By categorizing the extraction technology into seed and trichome, we examined and critiqued different pretreatment methods and technological options available for large-scale extraction in both categories. Solvent extraction methods being the main focus, the critical decision-making parameters in each stage, and the applicable current technologies in the field, were discussed. We further examined the factors affecting the cannabinoid transformation that changes the medical functionality of the final cannabinoid products. Based on the current trends, the extraction technologies are continuously being revised and enhanced, yet they still fail to keep up with market demands.
... • Required further separation process. Heleno et al. 2016Jadhav et al. 2009 Mechanical press • Simple and easy to operates • Higher yield ...
Article
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The demand for renewable energy has risen rapidly due to the depletion of petroleum oil. Biodiesel has attracted potential interest to be utilized as an alternative to petroleum oil since it is produced from renewable resources with minimal environmental impact. However, the production and quality of biodiesel potentially influence several factors including physicochemical properties of lipids, selection of feedstock, and technology utilized for lipids extraction. Candlenut contains the highest amount of oil among the oilseed crops. Supercritical carbon dioxide (scCO2) is viewed as an effective alternative method over conventional solvent extraction methods for the extraction and separation of lipids from various plant matrices. The distinct properties of the fluid CO2, such as nonflammability, nontoxicity, environmental friendliness, and its ability to solubilize lipophilic substance led to the wide application of the scCO2 in various industrial applications. Hence, the present study attempts to review the influence of the supercritical carbon dioxide (scCO2) technology for the extraction of lipids from candlenut as a potential feedstock for biodiesel production. The limitations of existing technologies in candlenut oil extraction and the potential scCO2 technology for the extraction of lipids from candlenut were also reviewed.
... However, this technology is expensive in terms of capital and operational expenditures, due to both the required equipment and operational conditions. On the other hand, Conventional Soxhlet extraction [17] requires a small amount of organic solvents; however, this separation technology requires long operation times and high energy consumption. Other studies use microwave-assisted extraction to recover vanillin [18], which reduce extraction time, but may degrade vanillin at high temperatures [19]. ...
Article
This paper presents an experimental and theoretical study for a perstraction system to recover diluted vanillin from aqueous solutions using an organophilic and hydrophobic membrane of polydimethylsiloxane (PDMS), and the hydrophobic ionic liquids (ILs) 1-butyl-3-methylimidazolium bis((trifluoromethyl)sulfonyl)imide ([bmim][Tf2N]), 1-octyl-3-methylimidazolium bis((trifluoromethyl)sulfonyl)imide ([omim][Tf2N]) and trihexyl tetradecyl phosphonium cyanamide ([P6,6,6,14][DCA]) as the extractant phase. The proposed mass transfer model was established as suitable for describing the extraction of vanillin from the aqueous phase in the perstraction system using ILs. According to this model, it was determined that the main mass transfer resistances were offered by the PDMS membrane, followed by the IL. [P6,6,6,14][DCA] experimentally showed a 13% increase in the transmembrane flux in comparison with the [Tf2N] anion based ILs, but also showed higher water transmembrane flux. In this regard, [omim][Tf2N] was found to exhibit better vanillin/water selectivity. The perstraction system gives better transmembrane fluxes than the data reported in the literature for vanillin extraction using pervaporation system. On the other hand, according to the screening in COSMO-RS, the combination of the anions DCA, SCN, TCC, Otf, PFBS, Tf2N, Pf2N y PF6 with pyrrolidinium, piperidinium and phosphonium base cations, are suitable to increase the performance of vanillin extraction.
... According to Fig. 9, the hydrogels maintained an significant coloration after being placed in the aqueous solution for 24 h and the aqueous solution had no obvious colour change by UV irradiation, indicating that SPBU-PEG had excellent stability in solution because of the microporous structure of the hydrogels that can restrain SPBU well and the hydrophobicity of the SPBU molecule itself. According to Table S2, the gel contents represented that the as-prepared SPBU-PEG hydrogels had preferable stability and high cross-linking degree [58]. ...
Article
How to detect and recover Cr(III) (Cr³⁺) from contaminated water through an economical and environmental way is not negligible but significant to solve serious pollution of heavy metal ions. Herein, a spiropyran [1′-(n-butyl)-3′,3′-dimethyl-6-nitrospir[chromene-2,2′-indoline] (SPBU) with negative photochromism is exploited as a visual detector for Cr³⁺. In contrast to positive photochromism of spiropyran derivatives, the synthesized SPBU can isomerize from colorless form spiropyran (SP) to the corresponding colored merocyanine (MC) form and further complex with Cr³⁺ under darkness without essential UV irradiation, providing a facile strategy enable visual detection of Cr³⁺ in aqueous solution. Importantly, we have synthesized SPBU-Polyethylene glyol (SPBU-PEG) hydrogels with negative photochromism via physical blending. Evidence from practical performance confirms that Cr³⁺ can be captured from aqueous solution under darkness and repelled from the hydrogel effectively upon visible light irradiation to achieve the regeneration of the designed adsorbent with a save-energy manner, avoiding any desorbent and secondary contamination. Additionally, the SPBU-PEG hydrogels have excellent Cr³⁺ selectivity and reproducibility. This work provides a significant greener way to exploit visible light responsive materials for reversible recovery of heavy metal ions from contaminated water with preferable performance, broadening sustainable development for purification systems.
... On the other hand, the production of one kg of vanillin requires approximately 500 kg of vanilla pods, which depends on approximately 40,000 hand pollinated flowers (Ciriminna et al. 2019). Due to its irreplaceable characteristic fragrance, vanillin has occupied a prominent place in various food products, beverage, perfumery, pharmaceuticals, and cosmetic industries (Jadhav et al. 2009). Thus, extensive cultivation is needed to satisfy the increasing global demand for natural vanilla flavor. ...
Article
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An advanced micropropagation protocol has been developed for the global spice crop Vanilla planifolia using meta-topolin [mT, 6-(3-hydroxybenzylamino) purine] for the first time. Among the two types of cytokinins [mT and BAP (6-benzylaminopurine)] experimented, healthy shoot development and growth in terms of shoot numbers (5.0 ± 0.20/explant) with shoot length (4.3 ± 0.17 cm) were noted on agar-gelled Murashige and Skoog’s (MS) medium supplemented with 1.0 mg L−1 mT. The regenerated shoots were multiplied in liquid medium using the continuous shake-flask culture method in an incubator shaker. The liquid MS medium containing 0.5 mg L−1 mT + 0.25 mg L−1 α-Naphthalene acetic acid (NAA) agitated at 60 rpm resulted in the production of 62.0 ± 0.31 shoots (3.8 ± 0.11 cm length) per explants per culture vessel after 3rd subculture, and this is the best rate of shoot proliferation among the prevailing reports on V. planifolia. Further, the transverse sections of the leaves revealed that the mT medium derived leaves were physically sturdy and physiologically more active with developed anatomical parameters, such as higher proportions of palisade and spongy parenchyma tissue, xylem and phloem elements, and abundant chloroplasts than the shoots raised on BAP. The leaves collected from the shoots of mT containing medium possessed the higher amount of chlorophylls (380.0 μg g−1 fresh weight) and carotenoids (52.0 μg g−1 fresh weight) under in vitro conditions. The concurrent ex vitro rooting and acclimatization method has been adopted to reduce the cost and time in large scale cloning of V. planifolia. All the shoots (100%) were rooted in soilrite™, when pulse treated with 100 mg L−1 NAA for 4 min. The ex vitro rooted plantlets were successfully acclimatized in a greenhouse. The regenerated clones’ genetic uniformity and stability with the donor plant were tested using Start codon targeted polymorphism and detected no somaclonal variation. All the plantlets were survived in the soil transplantation, confirming the production of genetically, physically, and physiologically stable plantlets of V. planifolia.
... Leaves were dried under shade and powdered. The powdered leaves were then extracted with methanol in a Soxhlet extraction apparatus (Macro Scientific Works, Delhi) following the protocol of Jadhav et al. 18 . Evaporation of the solvent followed by freeze drying (Heto Power Dry LL3000 Freeze Dryer; Thermo Fisher Scientific, India) yielded the crude dry extract. ...
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Phlogacanthus thyrsiflorus Nees is a medicinal herb commonly used in traditional folk medicine, and it is known to possess anticancer activity. Here, we explored the anticancer properties of methanolic extract of P. thyrsiflorus leaves in HeLa and MCF-7 cell lines. We observed nuclear fragmentation as indication of apoptosis in the MPT treated cancer cells using haematoxylin and eosin (H&E) as well as fluorescent dye. DNA from the treated cells showed characteristic laddering of DNA fragments in agarose gel electrophoresis. Cell populations undergoing secondary necrosis following apoptosis could also be detected in FACS by annexin V/propidium iodide (PI) staining. Activated caspase-3 in the treated HeLa cells was detected by polyclonal anti-caspase-3 antibody utilizing immunocytochemistry. Using transmission electron microscopy, sub-cellular changes like rough endoplasmic reticulum, swollen mitochondria, distorted mitochondrial membrane, loss of cristae and matrix were observed in the treated HeLa cells. Extensive plasma membrane blebbing was also observed by scanning electron microscopy. Our findings support that Phlogacanthus thyrsiflorus leaves are natural source of potent anticancer agent.
... Solvent resistance experiment was conducted via soaking a wafer sample in different solvent that was placed by a new solvent every day [34]. Gel contents were obtained by Soxhlet extraction experiment in THF at 90 • C [35]. The more details of characterization were supplied in Supporting Materials. ...
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... et al., 2008;Ma et al., 2009). The conventional methods have their own limitations such as low efficiency, lower yield and associated health hazards (Jadhav et al., 2009;Adje et al., 2010). The nonconventional extraction technique is Ultrasound-Assisted extraction (UAE) which involves the mixing of sample with organic solvents and placing it in ultrasounds for a specific time and temperature, the sound waves generate cavitation and rupture the cell wall of the sample resulting in extraction of phenolic compounds to the solvent medium (Da Porto et al.,2009). ...
... VPE was prepared according to the methodology of Jadhav et al. (2009) with slight modifications. Cured vanilla pods (10 g) were triturated in an electric grinder (A11 basic analytical mill, IKA) to form a paste which was suspended in 300 mL of ethanol for solvent assisted extraction for 24 h at room temperature, followed by filtration (Whatman filter paper no. ...
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Vanilla, a popular flavour extracted from Vanilla planifolia pods was tested for its antibiotic modulatory activity against extensively drug-resistant (XDR) Pseudomonas aeruginosa clinical isolates. Cured vanilla pod extract (VPE) was found non-bactericidal even at high doses (> 2000 µg/mL), however, it modulated the activity of several antibiotics at a sub-inhibitory concentration of 500 µg/mL. This modulation activity of VPE was observed for last line antibiotic options such as meropenem and tigecycline, as well as commonly used antibiotics like ciprofloxacin, levofloxacin and chloramphenicol. Further, it was observed that VPE inhibited the activity of efflux pumps in XDR P. aeruginosa clinical isolates. GC-MS spectral analysis revealed the dominance of vanillin, furfuran and some short-chain fatty acids in VPE. Therefore, further studies on the constituent ingredients in VPE are recommended to identify the active compounds and use them as antibiotic modulators and efflux pump inhibitors.
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The main purpose of this research article is to develop a vortex-assisted switchable hydrophilicity solvent liquid phase microextraction (VA-SHS-LPME) for the selective and efficient extraction of trace vanillin in food samples. Four switchable hydrophilicity solvents (SHSs) were prepared and tested for the extraction of vanillin. The obtained extract phase after phase separation was analyzed by UV-Vis spectrophotometry. The extraction parameters including pH, vortex time, NaOH volume, and SHS volume were optimized using central composite design based on response surface methodology. Under optimized conditions, the linear range (0.2-400 ng mL⁻¹ with r²=0.9985), limit of detection (0.06 ng mL⁻¹), limit of quantitation (2.0 ng mL⁻¹), extraction recovery (97±4%) and enhancement factor (220) were obtained. Also, relative standard deviations were less than 2.1% indicating good precision. The VA-SHS-LPME procedure showed some advantages including good extraction, low consumption of chemical and low matrix effect. Finally, the VA-SHS-LPME procedure was applied for the determination of vanillin in food samples, and acceptable recoveries (91±3–99±3%) were obtained.
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This review article points out, through an overview, aspects that are related to the procedures established by green analytical chemistry, for the extraction of bioactive compounds in plants, through the use of assisted techniques, as well as green solvents. Procedures that have less negative impact on the environment are being increasingly required for the extraction of biocompounds in the area of analytical chemistry due to aspects of sustainability, profitability and efficiency. To this end, green procedures aim to design environmentally benign chemical processes and synthetic methodologies, to eliminate or reduce the use of dangerous and toxic chemicals at any stage of production in industry or even in the laboratory. These extraction procedures will be defined as “green”, when using alternative solvents, reducing energy consumption, in addition to ensuring the safety and high quality of the extract. This review provides an overview of the green procedures applied and which had an effective action in the extraction of bioactive compounds in medicinal plants, supported thus by innovative, sustainable, and unconventional energy sources.
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Phenolic compounds are widely distributed among plant fruits. They are present in fruits, vegetables, nuts, seeds, leaves, flours, roots, beverages and their derivative products. Phenolic compounds present in foods include phenolic-acids, hydroxycinnamic-acids, phenylethanoids, flavonoids, anthocyanins, tannins and lignans along with their composition have been discussed. Literature showed that flavonoids and anthocyanins in fruits received greater attention as compared to other phenolic compounds.
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The need for naturally occurring pharmaceutical compounds has long been a topic of interest. Azadiractin is a naturally occurring biopesticide in margosa species. Green chemistry principles are employed to conserve valuable resources and minimize ill effects on the environment. The present study reports the ultrasound-assisted extraction of the total phenolic content from Azadirachta indica leaves. The Taguchi technique was employed to optimize factors affecting the yield of the total phenolic content such as particle size (0.15–0.60 mm), temperature (25–55 °C), the solid to liquid ratio (1:20–1:50 g mL⁻¹), and irradiation time (15–60 min). The statistical analysis revealed that particle size had the most significant effect on the yield, followed by temperature, irradiation time, and the solid to liquid ratio in that order. The optimized conditions resulted in a maximum yield of 30 milligram gallic acid equivalent per gram plant material of the total phenolic content. The rate constant and effective diffusivity were determined by the first-order kinetic model and Fick’s second law of diffusion, respectively. The effective diffusivity evaluated under optimized experimental conditions was 6.85 × 10⁻¹² m² s⁻¹.
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The coupling of innovative technologies has emerged as a smart alternative for the process intensification of bioactive compound extraction from plant matrices. In this regard, the development of hybridized techniques based on the low-frequency and high-power ultrasound and high-pressure technologies, such as supercritical fluid extraction, pressurized liquids extraction, and gas-expanded liquids extraction, can enhance the recovery yields of phytochemicals due to their different action mechanisms. Therefore, this paper reviewed and discussed the current scenario in this field where ultrasound-related technologies are coupled with high-pressure techniques. The main findings, gaps, challenges, advances in knowledge, innovations, and future perspectives were highlighted.
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A wide number of analytical terms have been applied erroneously for many years by analytical chemists, and they apply at present yet, by considering the time makes their use correct. The question is, may precedents validate the present use of incorrect scientific terms? Misused terms are found along the analytical process, starting for giving the name of sample to the exiguous fraction of the original sample that reaches the detector or the high‐resolution equipment after sample pretreatment and sample preparation. All the steps of the analytical process are considered in this article, with special emphasis on sample preparation and, within this, on the use of ultrasound, mainly for assisting extraction more unequivocally named as leaching or lixiviation. A call of attention in this respect is considered by the author to be of help to the analytical community. This article is protected by copyright. All rights reserved
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The growing demand for high added-value products, such as vanilla-derived compounds, and increasing environmental regulations make evident the need to find new sustainable solvents for extraction processes, which meet both legislative requirements and expected yields. Vanilla-derived compounds are known for their antioxidant and beneficial properties for human health. These compounds can be recovered from effluent streams, promoting decontamination and revaluation of wastewater. The potential of using neoteric solvents, i.e., biobased solvents and hydrophobic eutectic solvents, as an alternative to conventional volatile organic solvents, such as ethyl acetate, for sustainable recovery of vanilla-derived compounds through liquid-liquid extraction from aqueous environments was investigated. Three biobased solvents (2-methyltetrahydrofuran, cyclopentyl methyl ether, and d-limonene) and three hydrophobic eutectic solvents constituted by menthol and organic acids (1:1 dl-menthol:octanoic acid, 1:1 dl-menthol:decanoic acid, and 2:1 dl-menthol:dodecanoic acid) were evaluated. The extraction process was optimized in terms of the stirring time and solvent:feed volume ratio. The effect of the initial solute concentration was also analyzed. The extraction efficiency of solvents was determined by UV-visible spectrophotometry and high-performance liquid chromatography with diode-array detection. The experimental results indicated that 2-methyltetrahydrofuran yielded the highest extraction efficiency from a vanilla bean extract solution for both vanillin (95.37%) and vanillic acid (91.96%) with good repeatability (RSD < 0.40%). Regarding the rest of the neoteric solvents, cyclopentyl methyl ether and hydrophobic eutectic solvents provided extraction values between 31.6 and 95.4% for both vanilla-derived compounds, while d-limonene was significantly less effective. Finally, a solvent recycling and reuse study was successfully carried out, showing that 2-methyltetrahydrofuran stands out as a promising biobased extraction solvent for sustainable recovery of valuable vanilla constituents.
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This study endeavored to develop a method to evaluate the effect of ultrasound frequency on soybean protein extraction. In the ultrasonic frequencies range from 20 to 52 kHz, 28, 35, and 45 kHz were predicted to be the resonance frequencies in the ultrasound-assisted extraction (UAE) process of soybean protein by simulating the acoustic field distribution. The absolute sound pressure and the relative standard deviation could be well-coordinated via frequency regulation. The extraction experiment of soybean protein showed that the extraction rate was improved significantly (p < 0.05) with the aid of ultrasound. The extraction effect was optimal at 28 kHz and the extraction rate was improved to 73.35 g/100 g from 46.09 g/100 g of control under the same condition. The structure of the extracted protein was analyzed by the spectrum to further explore the mechanism of the effect of ultrasonic frequency. Spectral analysis showed that 20, 28, and 35 kHz had a significant influence on the structure of protein molecules. Therefore, acoustic field simulation can be used as one effective method for selecting ultrasonic frequency, which could help to optimize equipment and improve efficiency.
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In this study, the employment of aqueous enzymolysis using alcalase with ethanolic ultrasonication extraction method was investigated. The cordycepin content was analyzed by using reversed‐phase high‐performance liquid chromatography with a diode array detector. The result showed that the highest cordycepin content of 0.4365±0.0309 mg/g could be obtained under extraction conditions including total enzyme volume of 240 μL, incubation time of 50 min, incubation temperature of 55 °C, and ultrasonic power of 840 W. The comparative studies of antioxidant activities of the extract were determined in terms of the DPPH free radical scavenging assay, ferric ion reducing power assay, and H2O2 scavenging assay. Additionally, the MTT assay was conducted to evaluate the anticancer activities of the extract, illustrating the cytotoxic property against Hep‐G2 cancer cells with the half‐maximal inhibitory concentration (IC50) value of 12.20±0.03 μg/mL compared to that of 0.36±0.03 μg/mL for ellipticine, MCF‐7 cancer cells with the IC50 value of 11.60±0.09 μg/mL compared to that of 0.51±0.04 μg/mL for ellipticine, and Lu cancer cells with the IC50 value of 34.50±0.25 μg/mL compared to that of 0.32±0.03 μg/mL for ellipticine. This research illustrates the procedure of employing ultrasonication and enzymolysis assisted extraction method for cordycepin extraction from Vietnamese C. militaris. Various influential processing parameters such as pH, total enzyme volume, incubation time, incubation temperature, ultrasonic time, and ultrasonic power on cordycepin content were investigated to optimize the extraction process. Additionally, the extracts under optimal conditions were used to determine antioxidant and anticancer properties for futuristic uses as medicinal drugs.
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In this study, membrane based solvent extraction of vanillin as one of the most popular flavour was investigated theoretically using computational fluid dynamic technique. A mass transfer model and simulation was developed based on continuity and transport phenomena equations. The effect of operating parameters such as pH, type of solvent and feed flow rate as well as membrane specifications including fibres number, fibre length and porosity-to tortuosity ratio was investigated. There was good agreement between experimental data and modelling value in terms of vanillin extraction percentage. The results showed that butyl acetate is the best solvent and it had the highest vanillin extraction at pH of 7. It was found that increasing feed flow rate can decrease vanillin extraction due to reduction of residence time in the contactor. Change in the membrane specifications had positive impact on the vanillin extraction. Increase in all fibres length, number of fibre, and porosity-to tortuosity ratio because of improving residence time, mass transfer area, and increase in effective diffusivity, respectively led to the enhancement of vanillin extraction. The extraction was reached 44% when the fibre length became 5 times longer. Moreover, it was concluded that the membrane system showed better performance when the feed flows in the tube side of contactor.
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This review deals with the Vanilla plant: history; botanical description; chemistry of vanilla beans; curing of vanilla beans; commercial extraction of vanilla flavour; standard specifications and uses of vanilla flavour. The production of vanillin by both chemical and biotechnological methods is described. The biotechnological production of vanilla flavour metabolites by plant tissue/cell culture, microbial biotransformation and molecular approaches is also presented, together with a discussion on economic and safety considerations.© 2000 Society of Chemical Industry
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This paper presents a review of the ultrasonically assisted extraction of bioactive principles from herbs. Much of the work was carried out under European community grants under the COPERNICUS programme and in a COST D10 network. Some aspects of classical and non-conventional extraction procedures are also presented and briefly discussed.
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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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Vanilla, being the world's most popular flavoring materials, finds extensive applications in food, beverages, perfumery and pharmaceutical industry. With the high demand and limited supply of vanilla pods and the continuing increase in their cost, numerous efforts of blending and adulteration in natural vanilla extracts have been reported. Thus, to ensure the quality of vanilla extracts and vanilla-containing products, it is important to develop techniques to verify their authenticity. Quantitatively, vanillin is the major compound present in the vanilla pods and the determination of vanillin is a vital consideration in natural vanilla extracts. This paper provides a comprehensive account of different extraction processes and chromatographic techniques applied for the separation, identification and determination of chemical constituents of vanilla. The review also provides an account of different methods applied for the quantification and the authentification of chemical constituents of vanilla extract. As the various properties of vanilla are attributed to its main constituent vanillin, its physico-chemical and bioactive properties have also been outlined.
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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.
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This paper describes a simple and rapid HPLC technique for vanillin determination in alcohol vanilla extract. Vanillin was separated on a Nucleosil C18 column by using water and methanol (40:60) as the mobile phase and retention time was only 2.2min. The measurements were made by using a photodiode array detector of the most adequate maximum wavelength absorbance at 231nm. This method has been successfully applied for the determination of vanillin in some commercial extracts.
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The apparent specific volumes and the spin-spin relaxation times (T2 values) of diacetyl and vanillin, in ethanol-water binary solvent mixtures were determined in the concentration range 1–50% (ww) for solute and 0–100% (solvv) for ethanol in the binary mixture.The apparent specific volumes of diacetyl and vanillin showed a decrease with increasing concentration of solute and an increase with increasing concentration of ethanol in the binary solvent mixture. The former of these trends might be attributable to a hydrophobic stacking of the solute and to the effect of the formation of new solute-solvent intermolecular hydrogen bonds. The latter trend is marked only for low concentrations of solute, showing that the disturbance of water structure either by solute or by ethanol has an important effect on the apparent specific volume.Spin-spin relaxation times (T2 values) decreased with increasing concentration of solutes, as the proportion of ordered protons in solution increased (between solutions) and showed a minimum for the different concentrations of binary mixture (within solutions) which is attributed to the presence of ethanol in the binary mixture.The results for apparent specific volumes of diacetyl and vanillin, for the same range of concentrations, seem to be similar, reflecting similar packing characteristics of the two solutes. However, the slightly shorter T2 values of vanillin are an indication of the faster relaxation of the ring (unexchangeable) protons of this solute. These results are important for taste and flavour research.
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Vanilla beans from seven different vanilla growing regions of the world were analyzed for vanillin, p-hydroxybenzoic acid, p-hydroxybenzaldehyde, and vanillic acid. Beans were extracted to obtain singlefold extracts, and analysis was carried out using reversed-phase liquid chromatography. Analysis of the extracts, obtained from cured and uncured beans treated with beta-glucosidase, indicates that all of the above-mentioned compounds are present in green beans as glycosides and are released upon curing. In addition to glycosides of these four known monophenols, there are at least three other major glycosides in green vanilla beans which are hydrolyzed during the curing process.
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Acoustic and hydrodynamic cavitation can be used for a variety of applications ranging from biological applications such as cell disruption to chemical reactions such as oxidation of organic pollutants in aqueous effluents, including biorefractory toxic chemicals. Different equipment used for cavitational effects was compared based on a model reaction (decomposition of potassium iodide resulting into iodine liberation). A correlation was developed for the prediction of the cavitational yield in terms of the cavity collapse pressure. This correlation, when used with earlier correlations for the pressure amplitude generated during the violent collapse of cavities, will help design engineers to choose particular equipment, operating conditions, and geometric parameters to achieve a desired chemical change. The developed equation relating the macroscopic reaction rates with the collapse pressure is the first of its kind reported in the literature. Pilot-plant-scale hydrodynamic cavitation orifice plate setup is most energy-efficient, with significantly higher cavitational yields for the model reaction.
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The extraction of active principles or oils from vegetable products by means of an appropriate solvent is a classical unit operation in chemical engineering. The aim of the present work is to improve the yield or the selectivity of the extraction using ultrasound. Two solid–liquid extractions have been investigated: pyrethrines from pyrethrum flowers (Chrysanthemum cineraria) and oil from woad seeds (Isatis tinetoria). In the case of the first one, an acceleration of the kinetics and of the yield of the extraction has been obtained, probably linked to the increase of the intraparticular diffusion of the solute, which is the limiting step of mass transfer. On the other hand, ultrasound seems to have a weak effect in the case of woad seeds, probably because of the structure of the seeds. In order to distinguish the various effects acting on the ultrasound activation, a thermoelectric probe has been built for measuring the ultrasonic intensity profile. By this method, it is possible to investigate the influence of the presence of solid particles on the ultrasound wave propagation.
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Coconut is a tropical fruit largely consumed in many countries. In some areas of the Brazilian coast, coconut shell represents more than 60% of the domestic waste volume. The coconut shell is composed mainly of lignin and cellulose, having a chemical composition very similar to wood and suitable for phenolic extraction. In this work, the use of ultrasound to extract phenolic compounds from coconut shell was evaluated. The effect of temperature, solution to solid ratio, pH and extraction time were evaluated through a 2(4) experimental planning. The extraction process was also optimized using surface response methodology. At the optimum operating condition (30 degrees C, solution to solid ratio of 50, 15 min of extraction and pH 6.5) the process yielded 22.44 mg of phenolic compounds per gram of coconut shell.
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A novel strain of Bacillus fusiformis, producing high amounts of vanillin from isoeugenol, was isolated from soil. Using 60% (v/v) isoeugenol as substrate and solvent and at pH 4.0, 37 degrees C and 180 rpm, vanillin was produced at 32.5 g l(-1) over 72 h. The unused isoeugenol was reusable.
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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
The ultrasonic extraction (UE) of oil from the seeds of a semi-oriental tobacco (Nicotiana tabacum L.) plant strain by using n-hexane and petroleum ether was studied at different temperatures and seeds-to-solvent ratios. The oil yield depended on the seed comminution, the extraction temperature, the seeds-to-solvent ratio and the type of solvent. The oil yield was much higher if the seeds were ground before extraction. The oil yield increased with increasing the extraction temperature and with decreasing the seeds-to-solvent ratio. n-Hexane was somewhat more efficient in the oil extraction than petroleum ether. In recovering the tobacco seed oil (TSO), the UE was less efficient than the Soxhlet extraction. The advantage of the UE was a relatively high oil yield at 25 degrees C in a shorter time. The kinetics of UE of TSO was described using the model of unsteady diffusion through plant material.
Article
An ultrasonic method for the extractions of rutin and quercetin from Euonymus alatus (Thunb.) Sieb was investigated. The influence of four extraction variables on extraction yield of rutin and quercetin was discussed. The optimum extraction conditions found were: 70% aqueous ethanol; solvent: sample ratio 40:1 (v/w); extraction time 3 x 30 min. The recovery of rutin and quercetin and the reproducibility of the extraction method were determined. The optimized ultrasonic extraction conditions were applied to extract rutin and quercetin from dried stalks of E. alatus (Thunb.) Sieb. The application of sonication method was shown to be highly efficient in the extraction of rutin and quercetin from E. alatus (Thunb.) Sieb, compared with classical methods. The scanning electron microscopy (SEM) micrographs provided evidence of more rapid opening of plant cells treated by UAE in contrast to maceration.
Perfumery and Flavorings Synthesis Kirk-Othmer Encyclopedia of Chemical Technology
  • P Z Bedoukian
  • Usa Esposito
  • L J Formanek
  • K Kientz
  • G Mauger
  • F Maureaux
  • V Robert
  • G Truchet
Bedoukian, P.Z., 1986. Perfumery and Flavorings Synthesis, third ed. Allured Publishing, Wheaton, USA. Esposito, L.J., Formanek, K., Kientz, G., Mauger, F., Maureaux, V., Robert, G., Truchet, F., 1997. Kirk-Othmer Encyclopedia of Chemical Technology, fourth ed. John Wiley Sons, New York. pp. 812–825.
Perfumery and Flavorings Synthesis
  • P Z Bedoukian
Bedoukian, P.Z., 1986. Perfumery and Flavorings Synthesis, third ed. Allured Publishing, Wheaton, USA.
Kirk-Othmer Encyclopedia of Chemical Technology
  • L J Esposito
  • K Formanek
  • G Kientz
  • F Mauger
  • V Maureaux
  • G Robert
  • F Truchet
Esposito, L.J., Formanek, K., Kientz, G., Mauger, F., Maureaux, V., Robert, G., Truchet, F., 1997. Kirk-Othmer Encyclopedia of Chemical Technology, fourth ed. John Wiley Sons, New York. pp. 812-825.
A comprehensive review on vanilla flavor: extraction, isolation and quantification of vanillin and others constituents
  • A K Sinha
  • U K Sharma
  • N Sinha
Sinha, A.K., Sharma, U.K., Sinha, N., 2008. A comprehensive review on vanilla flavor: extraction, isolation and quantification of vanillin and others constituents. International Journal of Food Science Nutrition 59, 299-326.