Ultrasound-assisted extraction of three bufadienolides from Chinese medicine ChanSu

In this study, the application of ultrasound-assisted extraction (UAE) method was shown to be more efficient in extracting anti-tumor bufadienolides (bufalin, cinobufagin and resibufogenin) from important animal medicine of ChanSu than the maceration extraction (ME) and soxhlet extraction (SE) method. The effects of ultrasonic variables including extraction solvent, solvent concentration, solvent to solid ratio, ultrasound power, temperature, extraction time and particle size on the yields of three bufadienolides were investigated. The optimum extraction conditions found were: 70% (v/v) methanol solution, solvent to solid ratio of 10ml/g, ultrasound power of 125W, temperature of 20°C, extraction time of 20min and particle size of 60-80 mesh. The extraction yields of bufalin, cinobufagin and resibufogenin were 43.17±0.85, 52.58±1.12, 137.70±2.65mg/g, respectively. In order to achieve a similar yield as UAE, soxhlet extraction required 6h and maceration extraction required much longer time of 18h. The results indicated that UAE is an alternative method for extracting bufadienolides from ChanSu.     

Combining pressurized liquids with ultrasound to improve the extraction of phenolic compounds from pomegranate peel (Punica granatum L.)

The combination of ultrasound and pressurized liquid extraction (UAPLE) was evaluated for the extraction of phenolic compounds from pomegranate peels (Punica granatum L.). The influence of several variables of the process on extraction yield, including solvent type (water, ethanol + water 30, 50 and 70% v:v), temperature (50–100 °C), ultrasound power (0–800 W at the generator, or 0–38.5 W at the tip of the probe), mean particle size (0.68 and 1.05 mm), and number of cycles (1–5), were analyzed according to the yield of 20 different phenolic compounds. The most suitable temperatures for the extraction of phenolic compounds using water were from 70 to 80 °C. In general, 100 °C was not adequate since the lowest extraction yields were observed. Results suggested that ultrasound had a greater impact on extraction yields using large particles and that intermediate ultrasound power (480–640 W at the generator, or 23.1–30.8 W at the tip of the probe) produced the best results. Using small particles (0.68 mm) or large particles (1.05 mm), extraction with ultrasound was 1 cycle faster. Ultrasound may have offset the negative effect of the use of large particles, however, did not increase the yield of phenolic compounds in any of the cases studied after five cycles. Additionally, the continuous clogging problems observed with small particles were avoided with the use of large particles, which combined with ultrasound allowed consistent operation with good intra and inter-day reproducibility (>95%). Using samples with large particle size, the best extraction conditions were achieved with water extraction solvent, 70 °C extraction temperature, ultrasound power at 480 W, and 3 cycles, yielding 61.72 ± 7.70 mg/g. UAPLE demonstrated to be a clean, efficient and a green alternative for the extraction of phenolic compounds from pomegranate peels. These findings indicate that UAPLE has a great potential to improve the extraction of bioactive compounds from natural products.     

Sonoprocessing improves phenolics profile,antioxidant capacity,structure, and product qualities of purple corn pericarp extract

For the first time, purple corn pericarp (PCP) was converted to polyphenol-rich extract using two-pot ultrasound extraction technique. According to Plackett-Burman design (PBD), the significant extraction factors were ethanol concentration, extraction time, temperature, and ultrasonic amplitude that affected total anthocyanins (TAC), total phenolic content (TPC), and condensed tannins (CT). These parameters were further optimized using the Box-Behnken design (BBD) method for response surface methodology (RSM). The RSM showed a linear curvature for TAC and a quadratic curvature for TPC and CT with a lack of fit > 0.05. Under the optimum conditions (ethanol (50%, v/v), time (21 min), temperature (28 °C), and ultrasonic amplitude (50%)), a maximum TAC, TPC, and CT of 34.99 g cyanidin/kg, 121.26 g GAE/kg, and 260.59 of EE/kg, respectively were obtained with a desirability value 0.952. Comparing UAE to microwave extraction (MAE), it was found that although UAE had a lower extraction yield, TAC, TPC, and CT, the UAE gave a higher individual anthocyanin, flavonoid, phenolic acid profile, and antioxidant activity. The UAE took 21 min, whereas MAE took 30 min for maximum extraction. Regarding product qualities, UAE extract was superior, with a lower total color change (ΔE) and a higher chromaticity. Structural characterization using SEM showed that MAE extract had severe creases and ruptures, whereas UAE extract had less noticeable alterations and was attested by an optical profilometer. This shows that ultrasound, might be used to extract phenolics from PCP as it requires lesser time and improves phenolics, structure, and product qualities.     

Utilization of natural deep eutectic solvents and ultrasound-assisted extraction as green extraction technique for the recovery of bioactive compounds from date palm (Phoenix dactylifera L.) seeds: An investigation into optimization of process parameters

The green extraction of bioactive compounds from date seeds was investigated using seven natural deep eutectic solvents (NADES) coupled with ultrasound-assisted extraction (UAE). The seven NADESs mainly consisted of choline chloride as hydrogen bond acceptors (HBA) and four sugars, two organic acids, and one polyalcohol as hydrogen bond donors (HBD) were utilized in this study. When the extraction efficiency of the NADESs was compared to that of the conventional solvents, all the NADESs showed superior bioactive compounds recovery efficacy. The lactic acid-based NADES had the highest extraction efficiency and was further optimized using the response surface method and Box-Behnken design. A four-factors including extraction time (10, 20, and 30 min), ultrasound amplitude (70, 80, and 90 %), % NADES content (30 %, 50 %, and 70 %) and solid-to-solvent ratio (1:30, 1.5:30, and 2:30 g/ml) each at three levels (−1, 0 and 1) using Box-Behnken design was applied. The % NADES content and the solid-to-solvent ratio were the major factors influencing the extraction efficiency of the total phenolic content (TPC) and the 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity. The optimum extraction conditions included an extraction time of 15 min, ultrasound amplitude of 90 %, % NADES content of 70 % and solid-to-liquid ratio of 1:30 g/ml. The experimental values for TPC and DPPH at optimum extraction conditions were 145.54 ± 1.54 (mg GAE/g powder) and 719.19 ± 2.09 (mmol TE/g powder), respectively. The major phenolic compounds observed in the date seeds extracted using ChCl-LA were 3,4-dihydroxybenzoic acid, catechin and caffeic acid. This study reveals that the extraction of date seeds with NADES in combination with UAE technique was able to recover significantly higher amounts of phenolic compounds which could find useful applications in the food, pharmaceutical, and cosmetics industries.     

Effects of various factors of ultrasonic treatment on the extraction yield of all-trans-lycopene from red grapefruit (Citrus paradise Macf.)

The effects of various factors, including the extraction time, temperature, solvent/material ratio, the ultrasonic intensity and duty cycle of ultrasonic irradiation on the extraction yield of all-trans-lycopene from red grapefruit by ultrasound-assisted extraction (UAE) were investigated. In comparison with conventional solvent extraction (CSE), UAE showed a pronounced greater extraction yield and reduced extraction time effectively with a peak value at 30 min. The extraction yield was significantly influenced by temperature and the optimum condition was 30 °C. The extraction yield increased with increasing of solvent/material ratio until equilibrium was arrived at the optimal ratio of 3:1 (mL/g). The extraction yield increased first and then decreased with an increase in ultrasonic intensity. The extraction yield of UAE increased with the increase of duty cycle, whereas pulsed ultrasound with proper intervals was more efficient than continuous ultrasonication. The degradation via isomerisation of all-trans-lycopene under ultrasonic treatment was also observed with the formation of 9,13′-di-cis-, 9,13-di-cis-, 15-cis-, 13-cis- and 9-cis-lycopene isomers which were tentatively identified by HPLC-PAD.     

Development and validation of an efficient ultrasound assisted extraction of phenolic compounds from flax (Linum usitatissimum L.) seeds

Flaxseed accumulates in its seedcoat a macromolecular complex composed of lignan (secoisolariciresinol diglucoside, SDG), flavonol (herbacetin diglucoside, HDG) and hydroxycinnamic acids (p-couramic, caffeic and ferulic acid glucosides). Their antioxidant and/or cancer chemopreventive properties support their interest in human health and therefore, the demand for their extraction. In the present study, ultrasound-assisted extraction (UAE) of flaxseed phenolic compounds was investigated. Scanning Electron Microscopy imaging and histochemical analysis revealed the deep alteration of the seedcoat ultrastructure and the release of the mucilage following ultrasound treatment. Therefore, this method was found to be very efficient for the reduction of mucilage entrapment of flaxseed phenolics. The optimal conditions for UAE phenolic compounds extraction from flaxseeds were found to be: water as solvent supplemented with 0.2 N of sodium hydroxide for alkaline hydrolysis of the SDG–HMG complex, an extraction time of 60 min at a temperature of 25 °C and an ultrasound frequency of 30 kHz. Under these optimized and validated conditions, highest yields of SDG, HDG and hydroxycinnamic acid glucosides were detected in comparison to other published methods. Therefore, the procedure presented herein is a valuable method for efficient extraction and quantification of the main flaxseed phenolics. Moreover, this UAE is of particular interest within the context of green chemistry in terms of reducing energy consumption and valuation of flaxseed cakes as by-products resulting from the production of flax oil.     

Ultrasound-assisted extraction of saffron bioactive compounds; separation of crocins,picrocrocin, and safranal optimized by artificial bee colony

In this work, a four-factor five-level full factorial central composite design (CCD) was used to optimize the ultrasound-assisted extraction (UAE) of saffron major components, namely picrocrocin, safranal and crocin. The process parameters included ethanol concentration (0–100%), extraction time (2–10 min), duty cycle (0.2–1.0) and ultrasonic amplitude (20–100%). The extracted compounds were measured both by spectrophotometry and chromatography techniques. The results revealed that the middle concentrations of ethanol and relatively long process durations along with high duty cycles and ultrasonic amplitudes had the most profound impact on the yields of the extracted bioactives. UAE was optimized using response surface methodology (RSM) and artificial bee colony (ABC); a comparison between these methods indicated their optimization power was approximately the same. According to the RSM analysis, an ethanol concentration of 58.58%, extraction time of 6.85 min, duty cycle of 0.82 and amplitude of 91.11% were the optimum extraction conditions, while the optimal conditions resulting from ABC were 53.07%, 7.32 min, 0.93 and 100% for the UAE variables respectively. Finally, HPLC analysis was carried out on the UAE optimum extract resulting from RSM. Four crocetin esters were detected in the optimal extract.     

Ultrasound-assisted extraction of anthraquinones from roots of Morinda citrifolia

This study investigated the use of ultrasound-assisted extraction (UAE) to improve the extraction efficiency of the classical solvent extraction techniques such as maceration and soxhlet extraction to extract anti-oxidant activity compounds, anthraquinones, from the root of Morinda citrifolia. The effects of different extraction conditions were determined, i.e., temperature of (25, 45, 60 °C), ultrasonic power, solvent types, and compositions of ethanol in ethanol–water mixtures. The results show that the yield increases with increasing extraction times and extraction temperatures. The percent recovery of anthraquinones using ultrasound was found to be highly dependent on the type of solvents (acetone > acetonitrile > methanol > ethanol). Furthermore, the use of ethanol–water solution as extraction solvent increased the yield of anthraquinones due to the relative polarity, the swelling effect of plant tissue matrix by water, and increased sound absorption. To achieve the same recovery as that achieved by UAE, soxhlet extraction and maceration required much longer time.     

Intensification of extraction of curcumin from Curcuma amada using ultrasound assisted approach: Effect of different operating parameters

Curcumin, a dietary phytochemical, has been extracted from rhizomes of Curcuma amada using ultrasound assisted extraction (UAE) and the results compared with the conventional extraction approach to establish the process intensification benefits. The effect of operating parameters such as type of solvent, extraction time, extraction temperature, solid to solvent ratio, particle size and ultrasonic power on the extraction yield have been investigated in details for the approach UAE. The maximum extraction yield as 72% was obtained in 1 h under optimized conditions of 35 °C temperature, solid to solvent ratio of 1:25, particle size of 0.09 mm, ultrasonic power of 250 W and ultrasound frequency of 22 kHz with ethanol as the solvent. The obtained yield was significantly higher as compared to the batch extraction where only about 62% yield was achieved in 8 h of treatment. Peleg’s model was used to describe the kinetics of UAE and the model showed a good agreement with the experimental results. Overall, ultrasound has been established to be a green process for extraction of curcumin with benefits of reduction in time as compared to batch extraction and the operating temperature as compared to Soxhlet extraction.     

A novel strategy for producing nano-particles from date seeds and enhancing their phenolic content and antioxidant properties using ultrasound-assisted extraction: A multivariate based optimization study

Date seeds from the date palm fruit are considered as a waste and they are known to contain several bioactive compounds. Producing nanoparticles from the date seeds can enhances their effectiveness and their utilization as novel functional food ingredients. In this study, date seed nanoparticles (DSNPs) synthesized using acid (HCl) hydrolysis method (HCl concentration of 38% and hydrolysis time of 4 days) was found to have particle size between 50 and 150 nm. The obtained DSNPs were characterized by measuring particle size and particle charge (Zetasizer), morphology using scanning electron microscope (SEM), and determination of the functional groups using fourier-transform infrared spectroscopy (FTIR). DSNPs were further treated with green extraction technology [ultrasound-assisted extraction (UAE)] using water-based and methanol-based solvent for optimizing the extraction of the bioactive compounds by implementing response surface methodology (RSM). The UAE of DSNPs were analysed for set of responses including total phenolic content (TPC), total flavonoid content (TFC), 1,1-diphenyl-2-picrlthydrazyl (DPPH) radical scavenging activity, ferric ion reducing antioxidant power (FRAP), and 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radical scavenging activity. Three-factor and four-factor Box-Behnken design (BBD) of three models (Synthesis of DSNPs, UAE with water, and UAE with methanol) was performed. The results showed that in UAE of DSNPs using water-based solvent, the key independent factors effecting the TPC and TFC and antioxidant activities were S:L ratio (40:1 mg/ml) and treatment time (9 min). Whereas the methanol-based UAE of DSNPs was mostly affected by US amplitude/power (90%) and methanol concentration (80%). All models were further optimized using response optimizer in Minitab and the generated predicted values were very comparable to the actual obtained results which confirm the significance and validity of all RSM models used. The phenolic compounds identified from DSNPs consisted mainly of 3,4-Dihydroxy benzoic acid, ferulic acid, and p-coumaric acid. The present study demonstrated a successful method for synthesising DSNPs as well as documented the optimum UAE conditions to maximize the extraction of polyphenolic compounds from DSNPs and enhancing their antioxidant activities to be used in food application.     

Extraction of bioactive compounds from defatted passion fruit bagasse (Passiflora edulis sp.) applying pressurized liquids assisted by ultrasound

Passion fruit bagasse is a rich source of phenolic compounds, including piceatannol, a stilbene to which several biological activities are conferred. This work reports the application of pressurized liquid extraction (PLE) assisted by ultrasound (US) to intensify the extraction of phenolic compounds from defatted passion fruit bagasse (DPFB). PLE at different temperatures (65–75 °C) without and with different US powers (240–640 W) was performed to investigate the mechanism of the assisted process. The extracts were evaluated in terms of global, total phenolic (TP), piceatannol and total reducing sugar yields. The antioxidant capacity of the extracts was determined by FRAP and ORAC assays. PLE assisted by US increased the yields, resulting in 60% more TP and piceatannol. The observed yields suggest that the main mechanism driving PLE assisted by US from DPFB was the rise in temperature caused by the ultrasonic waves. Pearson coefficient revealed a strong correlation between antioxidant capacity and total phenolics and piceatannol yield. The three-line spline model was adequately fitted to the experimental curves, showing three extraction periods in which the recovery of TP and piceatannol was higher than 70% at the end of the falling extraction rate period. PLE assisted or not by US showed to be clean, efficient and green alternatives for the recovery of phenolic compounds. The findings of this work indicate that PLE assisted by US has a great potential to improve the extraction of bioactive compounds from natural products.     

Ultrasound-assisted extraction of hesperidin from Penggan (Citrus reticulata) peel

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.     

Ultrasound pretreatment of wheat dried distiller’s grain (DDG) for extraction of phenolic compounds

Wheat Dried distiller’s grain (DDG), a coproduct from the ethanol production process, is rich in potentially health-promoting phenolic compounds. In the extraction of phenolic compounds from DDG, the DDG cell wall is an important barrier for mass transfer from the inside to the outside of the cell. The effect of high-power ultrasound pretreatment on destruction of DDG cell walls and extraction yield and rate was investigated. Direct sonication by an ultrasound probe horn at 24 kHz was applied and factors such as ultrasound power and treatment time were investigated. The method of nitrogen (N₂) adsorption at 77 K was used as a means to determine and compare the changes in physical properties (specific surface area, pore volume and pore size) of the treated samples at different levels of ultrasound power and treatment time. Increasing specific surface area, pore volume and pore size caused by ultrasonic treatment implied development of new or larger pores and damaged cell walls. Also, it was observed that the ultrasound pretreatment of DDG particles increased the extraction yield and rate of phenolic compounds from DDG by 14.29%. Among tested ultrasound conditions, 100% ultrasound power for 30 s was evaluated as the best pretreatment condition.     

Influence of ultrasonic amplitude,temperature, time and solvent concentration on bioactive compounds extraction from propolis

An ultrasound assisted method was investigated to extract bioactive compounds from propolis. This method was based on a simple ultrasound treatment using ethanol as an extraction medium to facilitate the disruption of the propolis cells. Four different variables were chosen for determining the influence on the extraction efficiency: ultrasonic amplitude, ethanol concentration, temperature and time; the variables were selected by Box-Behnken design experiments. These parameters were optimised in order to obtain the highest yield, and the results exhibited the optimum conditions for achieving the goal as 100% amplitude of ultrasonic treatment, 70% solvent concentration, 58 °C and 30 min. The extraction yield under modified optimum extraction conditions was, as follows: 459.92 mg GAE/g of TPC, 220.62 mg QE/g of TFC and 1.95% of balsam content. The results showed that the ultrasound assisted extraction was suitable for bioactive compounds extraction from propolis. The most abundant phenolic compound was kaempferol (228.8 mg/g propolis) followed by myricetin (115.5 mg/g propolis), luteolin (27.2 mg/g propolis) and quercetin (25.2 mg/g propolis).     

Ultrasonically assisted acid extraction of manganese from slag

An ultrasonically assisted extraction (UAE) technique was developed for the extraction of manganese from electrolytic manganese slag using a sulfuric acid-hydrochloric acid mixture (4:0.3, v/v) as solvent. The UAE conditions were optimized and the significance of variables affecting UAE tested. The determination of manganese was carried out by atomic absorption spectrophotometry (AAS). The ultrasonic extraction efficiency of manganese can reach about 90% under the following optimum conditions: solvent-slag ratio: 4 mL/g; temperature: 333 K; particle size: 0.2 mm; extraction time: 35 min; amount of additive (citric acid): 8 mg/g slag. During the UAE process, the particle size parameter on the extraction was the most significant, followed by solvent-slag ratio, citric acid mass, time and temperature. The repeatability of UAE technique was satisfactory. The ultrasonic method shown to be a much superior approach to the conventional extraction method in the extraction of manganese from slag.     

Extraction of phenolics and anthocyanins from purple eggplant peels by multi-frequency ultrasound: Effects of different extraction factors and optimization using uniform design

In this work, multi-frequency ultrasound (working modes for the single-, dual- and tri-frequency in simultaneous ways) was applied to extract bioactive compounds from purple eggplant peels. The single-factor experiments were performed by varying six independent variables. A six-level-five-factor uniform design (UD) was further employed to evaluate the interaction effects between different factors. It was found that extraction temperature and extraction time significantly affected the total phenolic content (TPC), whereas the total monomeric anthocyanins (TMA) was mainly influenced by ethanol concentration, extraction temperature and solid-liquid ratio. Based on partial least-squares (PLS) regression analysis, the optimal conditions for TPC extraction were: 53.6 % ethanol concentration, 0.336 mm particle size, 44.5 °C extraction temperature, 35.2 min extraction time, 1:43 g/mL solid-liquid ratio, and similar optimal conditions were also obtained for TMA. Furthermore, the TPC and TMA extraction were investigated by ultrasound in different frequencies and power levels. Compared with single-frequency (40 kHz) and dual-frequency ultrasound (25 + 40 kHz), the extraction yield of TPC and TMA with tri-frequency ultrasound (25 + 40 + 70 kHz) increased by 23.65 % and 18.76 % respectively, which suggested the use of multi-frequency ultrasound, especially tri-frequency ultrasound, is an efficient strategy to improve the TPC and TMA extracts in purple eggplant peels.     

Comparison between the use of polyether ether ketone and stainless steel columns for ultrasonic-assisted extraction under various ultrasonic conditions

The ultrasound-assisted extraction (UAE) was conducted using the stainless steel (SS) and polyether ether ketone (PEEK) columns and analyzed with high-performance liquid chromatography (HPLC) to understand the mechanism of ultrasound-assisted chromatography (UAC). Empty SS and PEEK columns were used to extract dyes from a fabric under identical conditions with several parameters including the initial ultrasonic bath temperatures (30 °C and 40 °C), ultrasound power intensities (0, 20, 40, 60, 80, and 100 %), ultrasound operation modes (normal and sweep), and ultrasound frequencies (25 kHz, 40 kHz, and 132 kHz) to compare their extraction capabilities. After 30 min of extraction, the amount of extract was determined by HPLC. The PEEK material was significantly affected by ultrasonic radiation compared to the SS material, especially at a higher temperature (40 °C), power intensity (100 %), and frequency (132 kHz) with sweep mode. At a maximum power density of 45 W/L, the extraction effectiveness ratio of PEEK to SS was in the range of 1.8 - 3.9 depending on the specific frequency, initial temperature, and with or without temperature control. The most optimal ultrasound frequencies, in terms of enhancing extraction effectiveness, are in the order of 132 kHz, 40 kHz, and 25 kHz. Unlike the SS material, the PEEK material was more affected by temperature and acoustic effects under identical conditions, especially at 132 kHz ultrasound frequency. In contrast, at lower frequencies of 40 kHz and 25 kHz, no significant differences in the acoustic effects were observed between the PEEK and SS materials. The findings of this study contribute to elucidating the roles of column materials in UAE and UAC.     

Optimization and comparison of ultrasound/microwave assisted extraction (UMAE) and ultrasonic assisted extraction (UAE) of lycopene from tomatoes

The extracting technology including ultrasonic and microwave assisted extraction (UMAE) and ultrasonic assisted extraction (UAE) of lycopene from tomato paste were optimized and compared. The results showed that the optimal conditions for UMAE were 98 W microwave power together with 40 KHz ultrasonic processing, the ratio of solvents to tomato paste was 10.6:1 (V/W) and the extracting time should be 367 s; as for UAE, the extracting temperature was 86.4 °C, the ratio of the solvents to tomato paste was 8.0:1 (V/W) and the extracting time should be 29.1 min, while the percentage of lycopene yield was 97.4% and 89.4% for UMAE and UAE, respectively. These results implied that UMAE was far more efficient extracting method than UAE.     

Optimization of ultrasonic-assisted extraction of pomegranate (Punica granatum L.) seed oil

The effectiveness of ultrasonic-assisted extraction (UAE) of pomegranate seed oil (PSO) was evaluated using a variety of solvents. Petroleum ether was the most effective for oil extraction, followed by n-hexane, ethyl acetate, diethyl ether, acetone, and isopropanol. Several variables, such as ultrasonic power, extraction temperature, extraction time, and the ratio of solvent volume and seed weight (S/S ratio) were studied for optimization using response surface methodology (RSM). The highest oil yield, 25.11% (w/w), was obtained using petroleum ether under optimal conditions for ultrasonic power, extraction temperature, extraction time, and S/S ratio at 140 W, 40 °C, 36 min, and 10 ml/g, respectively. The PSO yield extracted by UAE was significantly higher than by using Soxhlet extraction (SE; 20.50%) and supercritical fluid extraction (SFE; 15.72%). The fatty acid compositions were significantly different among the PSO extracted by Soxhlet extraction, SFE, and UAE, with punicic acid (>65%) being the most dominant using UAE.     

Bio-refinery of orange peels waste: A new concept based on integrated green and solvent free extraction processes using ultrasound and microwave techniques to obtain essential oil,polyphenols and pectin

In this study, extraction of essential oil, polyphenols and pectin from orange peel has been optimized using microwave and ultrasound technology without adding any solvent but only “in situ” water which was recycled and used as solvent. The essential oil extraction performed by Microwave Hydrodiffusion and Gravity (MHG) was optimized and compared to steam distillation extraction (SD). No significant changes in yield were noticed: 4.22 ± 0.03% and 4.16 ± 0.05% for MHG and SD, respectively. After extraction of essential oil, residual water of plant obtained after MHG extraction was used as solvent for polyphenols and pectin extraction from MHG residues. Polyphenols extraction was performed by ultrasound-assisted extraction (UAE) and conventional extraction (CE). Response surface methodology (RSM) using central composite designs (CCD) approach was launched to investigate the influence of process variables on the ultrasound-assisted extraction (UAE). The statistical analysis revealed that the optimized conditions of ultrasound power and temperature were 0.956 W/cm² and 59.83 °C giving a polyphenol yield of 50.02 mg GA/100 g dm. Compared with the conventional extraction (CE), the UAE gave an increase of 30% in TPC yield. Pectin was extracted by conventional and microwave assisted extraction. This technique gives a maximal yield of 24.2% for microwave power of 500 W in only 3 min whereas conventional extraction gives 18.32% in 120 min. Combination of microwave, ultrasound and the recycled “in situ” water of citrus peels allow us to obtain high added values compounds in shorter time and managed to make a closed loop using only natural resources provided by the plant which makes the whole process intensified in term of time and energy saving, cleanliness and reduced waste water.