Optimization of ultrasound-assisted extraction (UAE) of flavonoids compounds (FC) from hawthorn seed (HS)

Hawthorn seed (HS), an important by-product of the Hawthorn industry, is rich in potentially health-promoting flavonoids compounds. In this paper, the ultrasound-assisted extraction (UAE) of FC from HS was investigated. Important variables and their levels were obtained using Plackett-Burman (PB) design and Box-Behnken (BB) design. A mathematical model was developed to show the effects of each variable and their combinatorial interactions on extraction yield of FC. A high coefficient of determination (R² = 91.26%) indicated good agreement between the experimental and predicted values of FC yield. The optimum levels of these significant parameters were determined using response surface methodology (RSM), which revealed these as follows: ultrasound temperature 65 °C, ultrasonic time 37 min, extraction temperature 91 °C, extraction time 1.5 h, solid-liquid ratio of 1:18, and 72% ethanol. Under the optimum condition, the UAE rate of FC was up to 91.7%, and the yield of FC was 16.45 ± 0.02 mg/g (P < 0.05) that was 1.32-fold the yield of conventional reflux extraction (CRE).     

Optimization of ultrasound assisted extraction of antioxidant compounds from marjoram (Origanum majorana L.) using response surface methodology

The present study optimized the ultrasound assisted extraction (UAE) conditions to maximize the antioxidant activity [Ferric ion Reducing Antioxidant Power (FRAP)], total phenol content (TP) and content of individual polyphenols of extracts from marjoram. Optimal conditions with regard to amplitude of sonication (24.4-61.0 μm) and extraction temperature (15-35 °C) and extraction time (5-15 min) were identified using response surface methodology (RSM). The results showed that the combined treatment conditions of 61 μm, 35 °C and 15 min were optimal for maximizing TP, FRAP, rosmarinic acid, luteolin-7-O-glucoside, apigenin-7-O-glucoside, caffeic acid, carnosic acid and carnosol values of the extracts. The predicted values from the developed quadratic polynomial equation were in close agreement with the actual experimental values with low average mean deviations (E%) ranging from 0.45% to 1.55%. The extraction yields of the optimal UAE were significantly (p < 0.05) higher than solid/liquid extracts. Predicted models were highly significant (p < 0.05) for all the parameters studied with high regression coefficients (R²) ranging from 0.58 to 0.989.     

Direct enrichment of olive oil in oleuropein by ultrasound-assisted maceration at laboratory and pilot plant scale

The possibility to improve the nutritional value of olive oil by enriching it in phenolic compounds from olive leaves (e.g., oleuropein) by ultrasonic maceration was studied. The experimental design used led to the following optimal extraction conditions: ultrasonic power of 60 W, temperature of 16 °C and sonication duration of 45 min. The high total phenolic content (414.3 ± 3.2 mg of oleuropein equivalent/kg of oil), oleuropein (111.0 ± 2.2 mg/kg of oil) and α-tocopherol (55.0 ± 2.1 g/kg of oil) concentrations obtained by optimized ultrasound-assisted extraction (UAE) proved the efficiency of this process when compared with the conventional solid-liquid extraction. Histochemical analyses showed that this efficiency is due to specific alteration of the phenol-containing leaf structures. Furthermore, the radical-scavenging activity of the processed oil (DPPH test) and its stability toward lipid autoxidation (heating test) confirmed its enrichment in antioxidants. Sensory evaluation of the enriched olive oil showed a slight increase in bitterness but an overall acceptability. Finally, the enriched olive oil was characterized by clear green color (L^∗, a^∗, b^∗ parameters).     

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.     

UAE, MAE, SFE-CO2 and classical methods for the extraction of Mitragyna speciosa leaves

Mitragyna speciosa, a tropical plant indigenous to Southeast Asia, is well known for its psychoactive properties. Its leaves are traditionally chewed by Thai and Malaysian farmers and manual labourers as it causes a numbing, stimulating effect. The present study aims to evaluate alkaloid yield and composition in the leaf extracts. For this purpose we have compared several non-conventional extraction techniques with classic procedures (room temperature or under heating). Dried M. speciosa leaves belonging to three batches of different origin (from Thailand, Malaysia and Indonesia) were extracted using ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE) and supercritical carbon dioxide extraction SFE-CO₂, using methanol, ethanol, water and binary mixtures. The extracts were compared using an HPLC/ESI-MS analysis of mitragynine and four other related alkaloids which were present in the alkaloid fraction. The extraction technique influences both the raw product yield and the relative alkaloid content of M. speciosa leaves. Of the several methods tested, MAE in a closed vessel at 110 °C (60 W, methanol/water 1:1) gave the highest alkaloid fraction amount, while UAE with an immersion horn at 25 °C (21.4 kHz, 50 W, methanol) showed the best yield for mitragynine.This work may prove to be a useful contribution to forensic, toxicological and pharmacognosy studies. Although the potential applications of M. speciosa alkaloids clearly need further investigation, these results may facilitate the scaling-up of their extraction.     

Optimization of the ultrasound-assisted extraction of melatonin from red rice (Oryza sativa) grains through a response surface methodology

An analytical ultrasound-assisted extraction (UAE) technique has been optimized and validated for the extraction of melatonin from rice grains. A Box–Behnken design in conjunction with a response surface methodology based on six factors and three levels was used to evaluate the effects of the studied factors prior to optimizing the UAE conditions. The significant (p < 0.05) response surface models with high coefficients of determination were fitted to the experimental data. Solvent composition and extraction temperature were found to have very significant effects on the response value (p < 0.005). The optimal UAE conditions were as follows: extraction time of 10 min, ultrasound amplitude of 30%, cycle of 0.2 s⁻¹, extraction temperature of 40 °C, 50% methanol in water as the extraction solvent at pH 3.5 and a solvent/solid ratio 2.5:1. The method validation ensured right values for linearity, LOD, LOQ, precision and recovery. Furthermore, the method was successfully applied in the analysis of a number of rice samples throughout the rice production process. Hence, it was demonstrated that this particular UAE method is an interesting tool for the determination of melatonin in rice grain samples.     

An ammonium sulfate/ethanol aqueous two-phase system combined with ultrasonication for the separation and purification of lithospermic acid B from Salvia miltiorrhiza Bunge

We studied the effect of ultrasonication extraction technology combined with ammonium sulfate/ethanol aqueous two-phase system (ATPS) for the separation of lithospermic acid B (LAB) from Salvia miltiorrhiza Bunge. According to the literature and preliminary studies, ammonium sulfate concentration, ethanol concentration, pH, ultrasonication power, ultrasonication time and the ratio of solvent-to-solid were investigated using a single factor design to identify the factors affecting separation. Taking into consideration a simultaneous increase in LAB recovery (R (%)) and partition coefficient (K), the best performance of the ATPS was obtained at 25 °C and pH 2 using ammonium sulfate 22% (w/w) and ethanol 30% (w/w). To keep the solvent-to-solid ratio at 10, response surface methodology was used to find the optimal ultrasonication power and ultrasonication time. Quadratic models were predicted for LAB yield in the upper phase. Optimal conditions of 572.1 W ultrasonication power and 42.2 min produced a maximum yield of LAB of 42.16 mg g⁻¹ sample. There was no obvious degradation of LAB with ultrasound under the applied conditions, and the experimental yield of LAB was 42.49 mg g⁻¹ sample and the purity was 55.28% (w/w), which was much higher than that obtained using conventional extraction. The present study demonstrated that ultrasound coupled with aqueous two-phase systems is very efficient tool for the extraction and purification of LAB from Salvia miltiorrhiza Bunge.     

Continuous and pulsed ultrasound-assisted extractions of antioxidants from pomegranate peel

There is a great demand for developing efficient extraction methods in order to reduce extraction time and increase the yield and activity of functional antioxidants. The yields, activities, and extraction kinetics of antioxidants from the dry peel of pomegranate marc were studied using ultrasound-assisted extraction in continuous and pulsed modes and the results were compared with conventional extraction (CE) at a temperature of 25 ± 2 °C and water/peel ratio of 50/1, w/w. The studied factors were intensity level and treatment time for continuous ultrasound-assisted extraction (CUAE), and intensity level, number of pulse repetition, and pulse duration and interval for pulsed ultrasound-assisted extraction (PUAE). The results showed that all factors significantly affected the antioxidant yield, but only treatment time had a significant effect on the antioxidant activity. Compared to CE, PUAE at an intensity level of 59.2 W/cm², and a pulse duration of 5 s and a resting interval of 5 s increased the antioxidant yield by 22% and reduced the extraction time by 87%. Similarly, CUAE at the same intensity level increased the antioxidant yield by 24% and reduced the extraction time by 90%. Since PUAE had 50% energy saving compared to CUAE, we recommend using PUAE for the extraction with antioxidant yield of 14.5% and DPPH scavenging activity of 5.8 g/g. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound-assisted extractions under PUAE and CUAE. This research clearly demonstrated the superiority of PUAE for producing antioxidants from peel of pomegranate marc.     

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.     

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.     

Ultrasound-assisted extraction of oleanolic acid and ursolic acid from Ligustrum lucidum Ait

Oleanolic acid and ursolic acid are the main bioactive compounds in fruit of Ligustrum lucidum Ait, which possess anti-inflammatory, antioxidative, antiprotozoal, antimutagenic and anticancer properties. In this study, the ultrasound-assisted extraction of oleanolic acid and ursolic acid from L. lucidum Ait was investigated with HPLC-photodiode array detection. Effects of several experimental parameters, such as type and concentration of extraction solvent, ratio of liquid to material, extraction temperature and extraction time, on extraction efficiencies of oleanolic acid and ursolic acid from L. lucidum were evaluated. The influence of experimental parameters on extraction efficiency of ursolic acid was more significant than that of oleanolic acid. The optimal extraction conditions were 95% ethanol, the ratio of material to liquid at 1:20, and extraction for 10 min at 40 °C under ultrasonic irradiation. Under the optimal conditions, the yields of oleanolic acid and ursolic acid were 6.3 ± 0.25 and 9.8 ± 0.30 mg/g, respectively. The results indicated that the ultrasound-assisted extraction is a very useful method for the extraction of oleanolic acid and ursolic acid from L. lucidum.     

Sequential extraction and enrichment of flavonoids from Euonymus alatus by ultrasonic-assisted polyethylene glycol-based extraction coupled to temperature-induced cloud point extraction

A green method for simultaneous extraction and enrichment of flavonoids from Euonymus alatus was developed by ultrasonic-assisted extraction (UAE) and temperature-induced cloud point extraction (TICPE) using PEG-base aqueous solution as the extractant. Based on screening different molecular weights of PEGs, PEG-400/water was used as the extractant, and the effects of key factors on extraction yields of flavonoids were investigated by single-factor experiments and response surface methodology (RSM). The optimum conditions of UAE were as follows: PEG-400 concentration of 16% (w/w), particle size of 80 mesh, solvent-to-material ratio of 60:1, extraction temperature of 90 °C and extraction time of 15 min. The results obtained by validation experiments were consistent with the values predicted by RSM. Temperature-induced formation of the aqueous two-phase system (ATPS) and TICPE process were further investigated by controlling temperature and adding (NH₄)₂SO₄. In the presence of (NH₄)₂SO₄, the ATPS formed at 75 ℃ and pH 3.5 could effectively improve separation and recovery of flavonoids with enrichment factor of above five times. Gallic acid, catechin, dihydromyricetin and ellagic acid in the extract were identified and confirmed by UPLC-Q-TOF-MS and the corresponding standards. The UAE-TICPE coupled to HPLC was successfully applied for extraction and determination of flavonoids in two batches of Euonymus alatus. The extraction yields of catechin, dihydromyricetin and total flavonoids were 0.377–0.684 mg/g, 1.091–1.353 mg/g and 2.612–3.146 mg/g, respectively. Compared to conventional extraction methods, PEG-based UAE integrated with TICPE in one-step procedure exhibited higher extraction efficiency and better extraction selectivity.     

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.     

The effect of high intensity focused ultrasound on luciferase activity on two tumor cell lines in vitro, under the control of a CMV promoter

In this study, we compared the effect of high intensity focused ultrasound (HIFU) and thermal stress on the luciferase activity, controlled by a cytomegaly virus (CMV) promoter in an in vitro model using two tumor cell lines (M21, SCCVII). HIFU was applied in a pulsed-wave mode with increasing voltage at constant pulse duration, or thermal stress was delivered over a range of temperatures (36-52 °C) for 5 min. The resulting luciferase activity was measured in live cells using a cooled CCD camera. Luciferase activity was measured at set time intervals over a total of 48 h post-stress. Compared to baseline, the luciferase activity of the M21 tumor cell line when exposed to HIFU was approximately 54.2 ± 67.5% (p < 0.01) higher at a temperature of 42 °C, and approximately 52.9±128.5% (p < 0.01) higher at 44 °C. In the SCCVII tumor cell line, the luciferase activity after HIFU application was 55.4 ± 66.6% (p < 0.01) higher compared to baseline at a temperature of 42 °C. The M21 and SCCVII tumor cell line when exposed to thermal stress alone did not increase the luciferase activity. M21 and SCCVII tumor cells exposed to HIFU showed a maximum decrease in cell viability to 45.3 ± 7.5% and 10.3 ± 7.5%, respectively, and when exposed to thermal stress to 85.3 ± 3.5% and 20.4 ± 6.5%, respectively, compared to the untreated control. In M21 and SCCVII cells exposed to HIFU, free radicals could be detected using the dichlorofluorescein dye. Our findings demonstrate that HIFU can enhance the luciferase activity controlled by a CMV promoter. However it also has a higher damaging effect on the cells.     

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.     

Investigation of in-plane orientation characteristics for Bi-2212/MgO thin films fabricated by the MOD method

We investigated the characteristics of in-plane orientation for c-axis-oriented Bi-2212 thin films on MgO substrates, fabricated by the metal–organic decomposition (MOD) method. Bi-2212/MgO films were annealed using a 2-step heat treatment. The dominant rotation angle of the Bi-2212 film was 45° ([1 0 0] of Bi-2212 // [1 1 0] of MgO) for a precursor film fabricated at 500 °C and fired at 840 °C for 0 min or 30 min. However, after firing for 1 h the ?-scanning signal indicating the 45° angle became smaller and the signal representing an angle of about ±12° ([1 0 0] of Bi-2212 // [5 1 0] of MgO) became larger. After firing for 3 h, this ±12° signal became dominant. The extent of the 45° angle’s shift to ±12° increased with increasing firing time. On the other hand, when the precursor film was fabricated at 430 °C, signals indicating angles of 0°, ∼±12°, and 45° were observed after firing for 30 min. The rotation angle depended on the precursor-fabrication temperature when the precursor film was fired at 840 °C for 0 min or 30 min.     

Combination of sonication and heating for metal extraction from inorganic fertilizers prior to microwave-induced plasma spectrometry determinations

This work reports a fast and efficient method for metal extraction in inorganic fertilizers by combining heating and sonication using an ultrasonic bath. Microwave-induced plasma optical emission spectrometry (MIP OES) was applied for the determination of Cd, Cu, Cr, Mn, Pb, and Zn in the extracts. Higher efficiency of metal extraction (∼100% for all metals except to Cd) was obtained for the treatment of 150 mg of fertilizer with 4 mL of 50% (v/v) HCl sonicated for 10 min and heating at 85 °C. Extractions applying only heating did not provide satisfactory results. The proposed procedure is simple and contributes to reduced production of waste in comparison to the official method.     

The sodium diffusion in aluminium-oxide

The transport of Na through the polycrystalline ceramic arc tube of high intensity discharge lamps has been investigated. This complex process consists of several steps: solution in the ceramics, diffusion through the ceramics, leaving the bulk phase, evaporation from the surface. Among the listed processes the kinetics of the diffusion was examined in the temperature range 400-1200 °C, separately from other disturbing effects. X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectroscopy (SIMS) were used to determine the concentration depth profiles. The obtained results confirmed that the grain boundary diffusion plays an important role in the transport process of sodium through the ceramic wall. The bulk and the grain boundary diffusion coefficients and the temperature dependencies of these transport processes have been determined. The activation energy of Na bulk diffusion is 56.5 ± 6.7 kJ/mol at 900-1200 °C, respectively the activation energies of Na grain boundary diffusion amount to 97.5 ± 21.6 kJ/mol in the temperature range 700-1100 °C and 7.7 ± 4.0 × 10⁻² kJ/mol at 400-700 °C. The preexponential factor of the bulk diffusion was found to be D_o = 5.1 × 10⁻¹⁵ ± 9.5 × 10⁻¹⁷ cm²/s in the temperature range 900-1200°C, whereas the preexponential factors of grain boundary diffusion are D_o = 1.1 × 10⁻¹⁰ ± 1.1 × 10⁻¹¹ cm²/s at 700-1100 °C and D_o = 7.5 × 10^-15 ± 1.5 × 10⁻¹⁷ cm²/s at 400-700 °C.     

Effect of plasma pretreatment on adhesion and mechanical properties of UV-curable coatings on plastics

An attempt was made to study the effect of plasma surface activation on the adhesion of UV-curable sol-gel coatings on polycarbonate (PC) and polymethylmethacrylate (PMMA) substrates. The sol was synthesized by the hydrolysis and condensation of a UV-curable silane in combination with Zr-n-propoxide. Coatings deposited by dip coating were cured using UV-radiation followed by thermal curing between 80 °C and 130 °C. The effect of plasma surface treatment on the wettability of the polymer surface prior to coating deposition was followed up by measuring the water contact angle. The water contact angle on the surface of as-cleaned substrates was 80° ± 2° and that after plasma treatment was 43° ± 1° and 50° ± 2° for PC and PMMA respectively. Adhesion as well as mechanical properties like scratch resistance and taber abrasion resistance were evaluated for coatings deposited over plasma treated and untreated surfaces.     

Optimisation of ultrasound assisted extraction of phenolic compounds from Sparganii rhizoma with response surface methodology

The present study reports on the extraction of phenolic compounds from sparganii rhizome. Box–Behnken Design (BBD), a widely used form of response surface methodology (RSM), was used to investigate the effect of process variables on the ultrasound-assisted extraction (UAE). Three independent variables including ethanol concentration (%), extraction time (min) and solvent-to-material ratio (mL/g) were studied. The results showed that the optimal UAE condition was obtained with an ethanol concentration of 75.3%, an extraction time of 40 min and a solvent-to-material ratio of 19.21 mL/g for total phenols, and an ethanol concentration of 80%, an extraction time of 33.54 min and solvent-to-material ratio of 22.72 mL/g for combination of ρ-hydroxybenzaldehyde, ρ-coumaric acid, vanillic acid, ferulic acid, rutin and kaempferol. The experimental values under optimal conditions were in good consistent with the predicted values, which suggested UAE is more efficient process as compared to solvent extraction.