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 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.     

Effect of oil extraction assisted by ultrasound on the physicochemical properties and fatty acid profile of pumpkin seed oil (Cucurbita pepo)

The effects of amplitude and time of ultrasound-assisted extraction on the physicochemical properties and the fatty acid profile of pumpkin seed oil (Cucurbita pepo) were evaluated. Ultrasound time (5–30 min) and the response variables amplitude (25–100%), extraction yield, efficiency, oxidative stability in terms of the free fatty acids (FFA) of the plant design comprising two independent experiments variables, peroxide (PV), p-anisidine (AV), totox value (TV) and the fatty acid profile were evaluated. The results were analyzed by multiple linear regression. The time and amplitude showed significant differences (P < 0.05) for all variables. The highest yield of extraction was achieved at 5 min and amplitude of 62.5% (62%). However, the optimal ultrasound-assisted extraction conditions were as follows: ultrasound time of 26.34 min and amplitude of 89.02%. All extracts showed low FFA (2.75–4.93% oleic acid), PV (1.67–4.68 meq/kg), AV (1.94–3.69) and TV (6.25–12.55) values. The main fatty acids in all the extracts were oleic and linoleic acid. Therefore, ultrasound-assisted oil extraction had increased performance and reduced extraction time without affecting the oil quality.     

Comparisons between conventional,ultrasound-assisted and microwave-assisted methods for extraction of anthraquinones from Heterophyllaea pustulata Hook f. (Rubiaceae)

This work reports a comparative study about extraction methods used to obtain anthraquinones (AQs) from stems and leaves of Heterophyllae pustulata Hook (Rubiáceae). One of the conventional procedures used to extract these metabolites from a vegetable matrix is by successive Soxhlet extractions with solvents of increasing polarity: starting with hexane to eliminate chlorophylls and fatty components, following by benzene and finally ethyl acetate. However, this technique shows a low extraction yield of total AQs, and consumes large quantities of solvent and time. Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) have been investigated as alternative methods to extract these compounds, using the same sequence of solvents. It was found that UAE increases the extraction yield of total AQs and reduces the time and amount of solvent used. Nevertheless, the combination UAE with benzene, plus MAE with ethyl acetate at a constant power of 900 W showed the best results. A higher yield of total AQs was obtained in less time and using the same amount of solvent that UAE. The optimal conditions for this latter procedure were UAE with benzene at 50 °C during 60 min, followed by MAE at 900 W during 15 min using ethyl acetate as extraction solvent.     

Novel utilization of waste marine sponge (Demospongiae) as a catalyst in ultrasound-assisted transesterification of waste cooking oil

This study demonstrates the potential of Na-silica waste sponge as a source of low cost catalyst in the transesterification of waste cooking oil aided by ultrasound. In this work an environmentally friendly and efficient transesterification process using Na-loaded SiO₂ from waste sponge skeletons as a solid catalyst is presented. The results showed that the methyl esters content of 98.4 ± 0.4 wt.% was obtainable in less than an hour (h) of reaction time at 55 °C. Optimization of reaction parameters revealed that MeOH:oil, 9:1; catalyst, 3 wt.% and reaction duration of 30 min as optimum reaction conditions. The catalyst is able to tolerant free fatty acid and moisture content up to 6% and 8%, respectively. In addition, the catalyst can be reused for seven cycles while maintaining the methyl esters content at 86.3%. Ultrasound undoubtedly assisted in achieving this remarkable result in less than 1 h reaction time. For the kinetics study at 50–60 °C, a pseudo first order model was proposed, and the activation energy of the reaction is determined as 33.45 kJ/mol using Arrhenius equation.     

Optimization of ultrasound-assisted extraction of total monomeric anthocyanin (TMA) and total phenolic content (TPC) from eggplant (Solanum melongena L.) peel

The present study describes the extraction of total monomeric anthocyanin (TMA) and total phenolic content (TPC) from eggplant peel using ultrasonic treatments and methanol and 2-propanol as extraction solvents. The extraction yields were optimized by varying the solvent concentration, ultrasonic frequency, temperature and time of ultrasonic treatment. Box–Behnken design was used to investigate the effect of process variables on the ultrasound-assisted extraction. The results showed that for TPC extraction the optimal condition were obtained with a methanol concentration of 76.6%, 33.88 kHz ultrasonic frequency, a temperature of 69.4 °C and 57.5 min extraction time. For TMA the optimal condition were the following: 54.4% methanol concentration, 37 kHz, 55.1 °C and process time of 44.85 min.     

Effects of ultrasound-assisted basic electrolyzed water (BEW) extraction on structural and functional properties of Antarctic krill (Euphausia superba) proteins

A novel protein extraction method of ultrasound-assisted basic electrolyzed water (BEW) was proposed, and its effects on the structural and functional properties of Antarctic krill proteins were investigated. Results showed that BEW reduced 30.9% (w/w) NaOH consumption for the extraction of krill proteins, and its negative redox potential (−800 ~ −900 mV) protected the active groups (carbonyl, free sulfhydryl, etc.) of the proteins from oxidation compared to deionized water (DW). Moreover, the ultrasound-assisted BEW increased the extraction yield (9.4%), improved the solubility (8.5%), reduced the particle size (57 nm), favored the transition of α-helix and β-turn to β-sheet, promoted the surface hydrophobicity and disulfide bonds formation of krill proteins when compared to BEW without ultrasound. These changes contributed to the enhanced foam capacity, foam stability and emulsifying capacity of the krill proteins. Notably, all the physicochemical, structural and functional properties of the krill proteins were comparable to those extracted by the traditional ultrasound-assisted DW. This study suggests that the ultrasound-assisted BEW can be a potential candidate to extract proteins, especially offering an alternative way to produce marine proteins with high nutritional quality.     

Multivariate optimization and comparison between conventional extraction (CE) and ultrasonic-assisted extraction (UAE) of carotenoid extraction from cashew apple

Carotenoids are an essential component of cashew and can be used in pharmaceuticals, cosmetics, natural pigment, food additives, among other applications. The present work focuses on optimizing and comparing conventional and ultrasound-assisted extraction methods. Every optimization step took place with a 1:1 (w:w) mixture of yellow and red cashew apples lyophilized and ground in a cryogenic mill. A Simplex-centroid design was applied for both methods, and the solvents acetone, methanol, ethanol, and petroleum ether were evaluated. After choosing the extractor solvent, a central composite design was applied to optimize the sample mass (59–201 mg) and extraction time (6–34 min). The optimum conditions for the extractor solvent were 38% acetone, 30% ethanol, and 32% petroleum ether for CE and a mixture of 44% acetone and 56% methanol for UAE. The best experimental conditions for UAE were a sonication time of 19 min and a sample mass of 153 mg, while the CE was 23 min and 136 mg. Comparing red and yellow cashews, red cashews showed a higher carotenoid content in both methodologies. The UAE methodology was ca. 21% faster, presented a more straightforward composition of extracting solution, showed an average yield of superior carotenoid content in all samples compared to CE. Therefore, UAE has demonstrated a simple, efficient, fast, low-cost adjustment methodology and a reliable alternative for other applications involving these bioactive compounds in the studied or similar matrix.     

The physical,mechanical, thermal and barrier properties of starch nanoparticle (SNP)/polyurethane (PU) nanocomposite films synthesised by an ultrasound-assisted process

This article reports on the ultrasound-assisted acid hydrolysis for the synthesis and evaluation of starch nanoparticles (SNP) as nanofillers to improve the physical, mechanical, thermal, and barrier properties of polyurethane (PU) films. During the ultrasonic irradiation, dropwise addition of 0.25 mol L^-1 H₂SO₄ was carried out to the starch dispersion for the preparation of SNPs. The synthesized SNPs were blended uniformly within the PU matrix using ultrasonic irradiation (20 kHz, 220 W pulse mode). The temperature was kept constant during the synthesis (4 °C). The nanocomposite coating films were made with a regulated thickness using the casting method. The effect of SNP content (wt%) in nanocomposite coating films on various properties such as morphology, water vapour permeability (WVP), glass transition temperature (Tg), microbial barrier, and mechanical properties was studied. The addition of SNP to the PU matrix increased the roughness of the surface, and Tg by 7 °C, lowering WVP by 60% compared to the PU film without the addition of SNP. As the SNP concentration was increased, the opacity of the film increased. The reinforcement of the SNP in the PU matrix enhanced the microbial barrier of the film by 99.9%, with the optimal content of SNP being 5%. Improvement in the toughness and barrier properties was observed with an increase in the SNP content of the film.     

Ultrasound-assisted extraction coupled with under vacuum distillation of flavour compounds from spearmint (carvone-rich) plants: Comparison with conventional hydrodistillation

Ultrasonically assisted extraction of flavour compounds from different varieties of Mentha spicata, using 70% ethanol, have been carried out for 5, 10 and 15 min and coupled with under vacuum distillation. The ultrasound distilled extracts have been analysed by GC–MS and compared with essential oils obtained by hydrodistillation. The results have showed that ultrasonically assisted extraction in combination with under vacuum distillation have provided extracts with higher flavouring strength due to the increased concentration of desirable oxygenated compounds (from 5 to 8 times) compared with hydrodistillation. Extraction yields of flavour volatiles have been calculated giving a range 0.04–0.13% by ultrasound and 0.01–0.02% by hydrodistillation.     

Ultrasonic-assisted extraction of polyphenolic compounds from Paederia scandens (Lour.) Merr. Using deep eutectic solvent: optimization,identification, and comparison with traditional methods

Ultrasonic-assisted extraction (UAE) coupled with deep eutectic solvent (DES) is a novel, efficient and green extraction method for phytochemicals. In this study, the effects of 16 DESs coupled with UAE on the extraction rate of polyphenols from Paederia scandens (Lour.) Merr. (P. scandens), an edible and medicinal herb, were investigated. DES synthesised with choline chloride and ethylene glycol at a 1:2 M ratio resulted in the highest extractability. Moreover, the effects of extraction parameters were investigated by using a two-level factorial experiment followed by response surface methodology The optimal parameters (water content in DES of 49.2%, the actual ultrasonic power of 72.4 W, and ultrasonic time of 9.7 min) resulted in the optimal total flavonoid content (TFC) (27.04 mg CE/g DW), ferric-reducing antioxidant power (FRAP) value (373.27 μmol Fe(Ⅱ)E/g DW) and 2,2′-azino-bis(3-ethylbenzthiazoline)-6-sulfonic acid radical (ABTS⁺) value (48.64 μmol TE/g DW), closely matching the experimental results. Furthermore, a comparison study demonstrated that DES-UAE afforded the higher TFC and FRAP value than traditional extraction methods. 36 individual polyphenolic compounds were identified and quantified by ultra-high-performance liquid chromatography-mass spectrometry (UHPLC-MS) in P. scandens extracts, and of which 30 were found in the extracts obtained by DES-UAE. Additionally, DES-UAE afforded the highest sum of individual polyphenolic compound content. These results revealed that DES-UAE enhanced the extraction efficiency for polyphenols and provided a scientific basis for further processing and utilization of P. scandens.     

Foodomics revealed the effects of ultrasonic extraction on the composition and nutrition of cactus fruit (Opuntia ficus-indica) seed oil

Cactus is a tropical fruit with a high nutritional value; however, little information is available regarding the comprehensive utilization of its byproducts. This study aimed to explore the composition and nutritional value of cactus fruit seed oil (CFO) and reveal the effects of ultrasound-assisted extraction and traditional solvent extraction on oil quality. Foodomics analysis showed that CFO extracted using a traditional solvent is rich in linolenic acid (9c12cC18:2, 57.46 ± 0.84 %), α-tocopherol (20.01 ± 1.86 mg/100 g oil), and canolol (200.10 ± 1.21 μg/g). Compared to traditional solvent extraction, ultrasound-assisted extraction can significantly increase the content of lipid concomitants in CFO, whereas excessive ultrasound intensity may lead to the oxidation of oils and the formation of free radicals. Analysis of the thermal properties showed that ultrasound had no effect on the crystallization or melting behavior of CFO. To further demonstrate the nutritional value of CFO, a lipopolysaccharide (LPS)-induced lipid metabolism imbalance model was used. Lipidomics analysis showed that CFO significantly reduced the content of oxidized phospholipids stimulated by LPS and increased the content of highly bioactive metabolites such as ceramides, thus alleviating LPS-induced damage in C. elegans. Hence, CFO is a functional oil with high value, and ultrasound-assisted extraction is advocated. These findings provide new insights into the comprehensive utilization of cactus fruits.     

Cu@SnS/SnO2 nanoparticles as novel sorbent for dispersive micro solid phase extraction of atorvastatin in human plasma and urine samples by high-performance liquid chromatography with UV detection: Application of central composite design (CCD)

Separation and detection of residual drug in biological fluids has directly related to human health in term of their beneficial or side effects. In biological fluid samples (complex matrix which containing drug at very low level) conduction of preliminary efficient technique as good choice for pre-concentration and clean-up of real sample before their instrumental analysis is highly recommended. In this result technique, based on nano-structure material which poses higher available surface area and larger member of reactive sites led to significant improvement in characteristic performance of analytical method. This paper focused on the synthesis and application of novel nano-sorbent for pre-concentration and extraction of atorvastatin (AT) from different biological fluids. Influence of various variables including sorbent dosage, eluent volume and sonication time on present method response was studied and optimized by central composite design under response surface methodology and accordingly an acceptable calibration curves over wide linear ranges (0.3–2000 μg L⁻¹) with high coefficient of determination higher than 0.999 strongly confirm high applicability of present method for quantification of analyte while limit of detection and quantification in plasma sample were 0.0608 and 0.2033 μg L⁻¹, respectively.     

Ultrasonically synthesis of Mn- and Cu- @ ZnS-NPs-AC based ultrasound assisted extraction procedure and validation of a spectrophotometric method for a rapid preconcentration of Allura Red AC (E129) in food and water samples

This study is devoted on Allura Red as food colorant preconcentration and determination in beverage, fruit juice and drink water samples is based on usage of Mn- and Cu- @ ZnS-NPs-AC as new sorbent for ultrasound-assisted-dispersive solid-phase microextraction (UA-DSPME) combined with ultraviolet–visible spectrophotometric based method (UV–Vis). Contribution of volume of eluent, pH, sorbent mass and sonication time on response following conduction of 28 experiments were optimized and investigated while their significantly justified according to p-value. Values of “Prob > F” less than 0.0500 is proportional with their significant influence on recovery of analyte. Under the optimum conditions 0.14 mL of THF; pH of 2.5; 8 mg of sorbent and 3 min sonication time guide and help achievement of limit of quantification (LOQ) and limit of detection (LOD) of 6.08 and 20.26 ng mL⁻¹, respectively. The accuracy of method was validated according to calculation of recovery following spiking 400 and 600 ng mL⁻¹ to blank solution and recovery as more reliable indication of accuracy 93.41 and 102.17% recoveries with RSD < 3.5%, which demonstrate the successful applicability of present method for real sample analysis. The maximum sorbent capacity was 50.0 mg g⁻¹ based on Langmuir isotherm as best model with high correlation coefficient. Combination of UA-DSPME and UV–Vis lead to higher sensitivity and lower cost for accurate and repeatable monitoring of Allura Red level in beverage, fruit juice and drink water samples with acceptable recovery and reasonable RSD%.