Influence of sequential exogenous pretreatment and contact ultrasound-assisted air drying on the metabolic pathway of glucoraphanin in broccoli florets

In this investigation, the combinations of exogenous pretreatment (melatonin or vitamin C) and contact ultrasound-assisted air drying were utilized to dry broccoli florets. To understand the influences of the studied dehydration methods on the conversion of glucoraphanin to bioactive sulforaphane in broccoli, various components (like glucoraphanin, sulforaphane, myrosinase, etc.) and factors (temperature and moisture) involved in the metabolism pathway were analyzed. The results showed that compared with direct air drying, the sequential exogenous pretreatment and contact ultrasound drying shortened the drying time by 19.0–22.7%. Meanwhile, contact sonication could promote the degradation of glucoraphanin. Both melatonin pretreatment and vitamin C pretreatment showed protective effects on the sulforaphane content and myrosinase activity during the subsequent drying process. At the end of drying, the sulforaphane content in samples dehydrated by the sequential melatonin (or vitamin C) pretreatment and ultrasound-intensified drying was 14.4% (or 26.5%) higher than only air-dried samples. The correlation analysis revealed that the exogenous pretreatment or ultrasound could affect the enzymatic degradation of glucoraphanin and the generation of sulforaphane through weakening the connections of sulforaphane-myrosinase, sulforaphane-VC, and VC-myrosinase. Overall, the reported results can enrich the biochemistry knowledge about the transformation of glucoraphanin to sulforaphane in cruciferous vegetables during drying, and the combined VC/melatonin pretreatment and ultrasound drying is conducive to protect bioactive sulforaphane in dehydrated broccoli.     

Simultaneous process optimization of ultrasound-assisted extraction of polyphenols and ellagic acid from pomegranate (Punica granatum L.) flowers and its biological activities

This study was designed to optimize the extraction rate of total polyphenols and ellagic acid from pomegranate flowers. Single factors were investigated for liquid-to-material ratio (5–25), ethanol concentration (20%–60%), sonication time (5–60 min), and sonication power (150–500 W). The level range of the Box-Bokhen design was determined with respect to the single-factor results. The components of each index were normalized using the entropy weighting method for obtaining the comprehensive evaluation value. Under the actual conditions, the final optimization results were 17 for liquid-to-material ratio, 43% for ethanol concentration, 10 min for ultrasonic time, and 300 W for ultrasonic power. The extracts obtained under optimal conditions were tested for the inhibition of Streptococcus mutans and its biofilm, and results showed that pomegranate flowers exerted some inhibitory effects on the bacterium. Phosphomolybdenum and FRAP assays were used, and DPPH, ABTS, and O²⁻ radical scavenging tests were conducted, indicating that pomegranate flower extracts have good antioxidant capacity.     

Ultrasonic-assisted extraction,fatty acids identification of the seeds oil and isolation of chemical constituent from oil residue of Belamcanda chinensis

Belamcanda chinensis is a common garden herb. The extraction technology of B. chinensis seed oil (BSO) was optimized by ultrasonic-assisted extraction (UAE) method, the composition, relative content of main fatty acids and physicochemical properties of BSO were determined, and the isolation, identification and determination of chemical constituent in BSO residue (BSOR) were also investigated. The optimum process conditions of BSO by UAE were optimized as ultrasound time 14 min, extraction temperature 42℃, the ultrasound power 413 W and the liquid–solid ratio 27:1 mL/g. Under this condition, the extraction yield was 22.32 % with the high contents of linoleic acid and oleic acid in BSO. Ten compounds were isolated and identified from BSOR, and belamcandaoid P (9) was a new compound. The contents of the determined compounds were all at high level in B. chinensis seed. The study provided a certain scientific reference for the comprehensive development and utilization of B. chinensis seeds.     

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.     

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.     

Comparison of ultrasound and microwave assisted extraction of diosgenin from Trigonella foenum graceum seed

From the recent market trend, there is a huge demand for the bioactive compounds from various food matrices that could be capable enough to combat the emerging health effects in day-to-day life. Fenugreek is a well-known spice from ancient times for its medicinal and health benefits. In the present study, two methods of green extraction microwave (MAE) and ultrasound (UAE) assisted were studied in regard of extraction of fenugreek diosgenin. In this study, solvent type (acetone, ethanol, hexane and petroleum ether), solvent concentration (40, 60, 80 and 100%) and treatment time (1.5, 3.0, 4.5 and 6.0 min and 30, 40, 50 and 60 min for MAE and UAE method respectively) was varied to observe the effect of these parameters over extract yield and diosgenin content. The results of this study revealed that treatment time, type of solvent and its concentration and method adopted for extraction of diosgenin has significant effect. In relation with better yield extract and diosgenin content, the yield of fenugreek seed extract was 7.83% with MAE and 21.48% with UAE of fenugreek seed powder at 80% ethanol concentration at 6 and 60 min respectively. The content of diosgenin was observed in fenugreek seed powder extract was 35.50 mg/100 g in MAE and 40.37 mg/100 g in UAE with 80% ethanol concentration at 6 and 60 min respectively. The overall range of yield of fenugreek extract was varied from 1.04% to 32.48% and diosgenin content was 15.82 mg/100 g to 40.37 mg/100 g of fenugreek seed powder including both extraction methods. This study revealed that UAE would impose better ways for preparing fenugreek extract and observing diosgenin content from fenugreek seeds.     

Ultrasonic assisted extraction of polyphenols from bayberry by deep eutectic supramolecular polymer and its application in bio-active film

Ultrasound and deep eutectic supramolecular polymers (DESP) is a novel combination of green extraction method for phytochemicals. In this study, a new type of green extractant was developed: DESP. It is a derivative of deep eutectic solvent (DES) and was prepared by supramolecular polymer unit β-cyclodextrin (β-CD) as hydrogen bond acceptor (HBA) and organic acid as hydrogen bond donor (HBD). The current work focuses on the use of ultrasonic-assisted (UAE) DESP extraction of polyphenolic compounds (PCs) from bayberry. The experimental results showed that DESP synthesized with β-CD and lactic acid (LA) in a ratio of 1:1 (w/w %) had the best extraction effect. And by using a three-level factor experiment and the response surface method, the predicted TPC content is very close to the actual content (28.85 ± 1.27 mg GAE/g). The DESP extract including PCs were further used as plasticizer for chitosan (CS) to prepare highly active green biofilms (DESP-CS). It is possible to reduce the tedious procedures for separating biologically active substances from DESP. The experiment proved that the prepared films have good mechanical properties, plastic deformation resistance, thermal stability and antioxidant activity.     

Bio-guided optimization of the ultrasound-assisted extraction of compounds from Annona glabra L. leaves using the etiolated wheat coleoptile bioassay

A bio-guided optimization of the extraction of bioactive components from Annona glabra leaves has been developed using the etiolated wheat coleoptile bioassay as the control method. The optimization of an ultrasound-assisted extraction of bioactive compounds using allelopathy results as target values has been carried out for the first time. A two-level fractional factorial experimental design was applied to optimize the ultrasound-assisted extraction. The solvent was the extraction variable that had the most marked effect on the resulting bioactivity of the extracts in the etiolated wheat coleoptile bioassay. Extraction time, extraction temperature and the size of the ultrasonic probe also influenced the bioactivity of the extracts. A larger scale extraction was carried out in the next step in the allelopathic study, i.e., the isolation of compounds from the bioactive extract and chemical characterization by spectroscopic techniques, including NMR. Eight compounds were isolated and identified from the active extracts, namely two steroids (β-sistosterol and stigmasterol), five diterpenes with the kaurane skeleton (ent-kaur-16-en-19-oic acid, ent-19-methoxy-19-oxokauran-17-oic acid, annoglabasin B, ent-17-hydroxykaur-15-en-19-oic acid and ent-15β,16β-epoxy-17-hydroxy-kauran-19-oic acid) and the acetogenin asimicin.The most active compound was annoglabasin B, which showed inhibition with values of −95% at 10⁻³ M, −87% at 5 × 10⁻⁴ M and greater than −70% at 10⁻⁴ M in the etiolated wheat coleoptile bioassay.     

Ultrasonic-enhanced surface-active ionic liquid-based extraction and defoaming for the extraction of psoralen and isopsoralen from Psoralea corylifolia seeds

Recently, integrated and sustainable methods for extracting active substances from plant materials using green solvents, i.e., ionic liquids, have gained increasing attention. Ionic liquids show superiority over conventional organic solvents; however, they also exhibit negative factors and problems, such as high viscosity, poor water intermiscibility, intensive foaming and poor affinity for fat-soluble substances. The proposed method utilizes ultrasonic-enhanced surface-active ionic liquid-based extraction and defoaming (UESILED) to improve the extraction efficiency of ionic liquids. Single-factor experiments and a Box-Behnken design (BBD) were utilized to optimize the extraction procedure. The optimal conditions were as follows: extraction solvent, [C₁₀MIM]Br; ultrasonic treatment time, 28 min; ultrasonic irradiation power, 437 W; liquid–solid ratio, 10 mL/g; particle size, 60 ~ 80 mesh; ultrasonication temperature, 313 K; and [C₁₀MIM]Br solution concentration, 0.5 mol/L. In comparison with those of other reference extraction methods, the proposed method exhibited higher yields of two furocoumarins and operational feasibility. Moreover, the mechanism of UESILED was elaborated in terms of accelerating infiltration, dissolution and defoaming. The feasible and efficient ultrasonic-enhanced ionic liquid-based extraction established in this study strongly contributes to overcoming the limitations of ionic liquid solvents. The present research indicates that this improved process will be beneficial for the extraction of other fat-soluble substances and provides promising concepts and experimental data.     

A possible general mechanism for ultrasound-assisted extraction (UAE) suggested from the results of UAE of chlorogenic acid from Cynara scolymus L. (artichoke) leaves

The use of ultrasound-assisted extraction (UAE) for the extraction of chlorogenic acid (CA) from Cynara scolymus L., (artichoke) leaves using 80% methanol at room temperature over 15 min gave a significant increase in yield (up to a 50%) compared with maceration at room temperature and close to that obtained by boiling over the same time period. A note of caution is introduced when comparing UAE with Soxhlet extraction because, in the latter case, the liquid entering the Soxhlet extractor is more concentrated in methanol (nearly 100%) that the solvent in the reservoir (80% methanol) due to fractionation during distillation. The mechanism of UAE is discussed in terms of the effects of cavitation on the swelling index, solvent diffusion and the removal of a stagnant layer of solvent surrounding the plant material.     

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.     

Optimisation of the ultrasound-assisted extraction of betalains and polyphenols from Amaranthus hypochondriacus var. Nutrisol

The present study optimised the ultrasound-assisted extraction (UAE) of bioactive compounds from Amaranthus hypochondriacus var. Nutrisol. Influence of temperature (25.86–54.14 °C) and ultrasonic power densities (UPD) (76.01–273.99 mW/mL) on total betalains (BT), betacyanins (BC), betaxanthins (BX), total polyphenols (TP), antioxidant activity (AA), colour parameters (L*, a*, and b*), amaranthine (A), and isoamaranthine (IA) were evaluated using response surface methodology. Moreover, betalain extraction kinetics and mass transfer coefficients (K_La) were determined for each experimental condition. BT, BC, BX, TP, AA, b*, K_La, and A were significantly affected (p < 0.05) by temperature extraction and UPD, whereas L*, a*, and IA were only affected (p < 0.05) by temperature. All response models were significantly validated with regression coefficients (R²) ranging from 87.46 to 99.29%. BT, A, IA, and K_La in UAE were 1.38, 1.65, 1.50, and 29.93 times higher than determined using conventional extraction, respectively. Optimal UAE conditions were obtained at 41.80 °C and 188.84 mW/mL using the desired function methodology. Under these conditions, the experimental values for BC, BX, BT, TP, AA, L*, a*, b*, K_La, A, and IA were closely related to the predicted values, indicating the suitability of the developed quadratic models. This study proposes a simple and efficient UAE method to obtain betalains and polyphenols with high antioxidant activity, which can be used in several applications within the food industry.     

Novel synthesis of nanocomposite for the extraction of Sildenafil Citrate (Viagra) from water and urine samples: Process screening and optimization

A sensitive analytical method is investigated to concentrate and determine trace level of Sildenafil Citrate (SLC) present in water and urine samples. The method is based on a sample treatment using dispersive solid-phase micro-extraction (DSPME) with laboratory-made Mn@ CuS/ZnS nanocomposite loaded on activated carbon (Mn@ CuS/ZnS-NCs-AC) as a sorbent for the target analyte. The efficiency was enhanced by ultrasound-assisted (UA) with dispersive nanocomposite solid-phase micro-extraction (UA-DNSPME). Four significant variables affecting SLC recovery like; pH, eluent volume, sonication time and adsorbent mass were selected by the Plackett-Burman design (PBD) experiments. These selected factors were optimized by the central composite design (CCD) to maximize extraction of SLC. The results exhibited that the optimum conditions for maximizing extraction of SLC were 6.0 pH, 300 μL eluent (acetonitrile) volume, 10 mg of adsorbent and 6 min sonication time. Under optimized conditions, virtuous linearity of SLC was ranged from 30 to 4000 ng mL⁻¹ with R² of 0.99. The limit of detection (LOD) was 2.50 ng mL⁻¹ and the recoveries at two spiked levels were ranged from 97.37 to 103.21% with the relative standard deviation (RSD) less than 4.50% (n = 15). The enhancement factor (EF) was 81.91. The results show that the combination UAE with DNSPME is a suitable method for the determination of SLC in water and urine samples.     

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.     

Comparison of hydrodistillation and ultrasonic solvent extraction for the isolation of volatile compounds from two unifloral honeys of Robinia pseudoacacia L. and Castanea sativa L

A comparative study of ultrasound-assisted extraction (USE) with the mixture pentane:ether (1:2) and hydrodistillation (HD) with the same trapping mixture is presented for the isolation of volatile compounds from two unifloral honeys of Robinia pseudoacacia L. and Castanea sativa L. All HD isolates contained many thermally derived artefacts (especially phenylacetaldehyde with lower percentages of furfural, cis- and trans-linalool oxides and others). USE method gave the most representative profile of all honey volatiles (without artefacts). In addition, USE enabled extraction of low molecular weight semivolatile markers (especially benzoic, vanillic and phenylacetic acids) that were not extracted by HD. In this regard, low percentage of benzoic acid (0.7–7.4%), vanillic acid (0.0–1.6%) and phenylacetic acid (0.5–4.1%) was determined in Rp USE extracts, while Cs USE extracts contained phenylacetic acid (20.2–23.5%) as the major constituent with low percentage of benzoic acid (2.5–5.5%).