Alternative green solvents associated with ultrasound-assisted extraction: A green chemistry approach for the extraction of carotenoids and chlorophylls from microalgae.

This study proposes a method for the ultrasonic extraction of carotenoids and chlorophyll from Scenedesmus obliquus and Arthrospira platensis microalgae with green solvents. Ethanol and ethanolic solutions of ionic liquids were tested with a variety of extraction parameters, including number of extractions, time of extraction, and solid-liquid ratio R(S/L), to determine the optimal conditions. After selecting the most effective green solvent (ethanol), the process conditions were established: R(S/L) of 1:10, three extraction cycles at 3 min each), giving an extraction yield of 2602.36 and 764.21 µgcarotenoids.gdried biomass-1; and 22.01 and 5.81 mgchlorophyll.gdried biomass-1 in S. obliquus and A. platensis, respectively. The carotenoid and chlorophyll extracts obtained using ethanol were shown to be potent scavengers of peroxyl radical, being 5.94 to 26.08 times more potent α-tocopherol. These findings pave the way for a green strategy for valorizing microalgal biocompounds through efficient and environmentally friendly technological processes.

Optimization of the Extraction Conditions of Bioactive Compounds from Ocimum basilicum Leaves Using Ultrasound-Assisted Extraction via a Sonotrode.

Sweet basil (Ocimum basilicum) leaves are rich in bioactive compounds that present therapeutic benefits for human health. Ultrasonic-assisted extraction (UAE) is frequently used to obtain phenolic compounds from plants/herbal sources. However, few works have developed multi-variable studies to find the optimal conditions to extract the maximum amount of compounds, especially when applied to UAE via a sonotrode. The purpose of this work was to perform a multi-variable study by employing a Box-Behnken design to collect the highest active compound content from Ocimum basilicum leaves. The efficacy of the design was endorsed by ANOVA. The studied parameters for UAE via a sonotrode were the ethanol/water ratio, amplitude, and time. The analyzed responses were the rosmarinic acid, the sum of phenolic acids, and the sum of phenolic compounds content. The optimal conditions were found to be 50% ethanol/water, 50% amplitude, and 5 min. Twenty bioactive compounds were identified by HPLC-ESI-TOF-MS when the extract was collected by applying the optimal conditions. Ocimum basilicum may be appreciated as a valuable source of important bioactive substances for pharmaceutical use.

Evaluation of the Biological Properties of an Optimized Extract of Polygonum cuspidatum Using Ultrasonic-Assisted Extraction.

Phytochemicals are natural compounds found in plants that have potential health benefits such as antioxidants, anti-inflammatory and anti-cancer properties, and immune reinforcement. Polygonum cuspidatum Sieb. et Zucc. is a source rich in resveratrol, traditionally consumed as an infusion. In this study, P. cuspidatum root extraction conditions were optimized to increase antioxidant capacity (DPPH, ABTS+), extraction yield, resveratrol concentration, and total polyphenolic compounds (TPC) via ultrasonic-assisted extraction using a Box-Behnken design (BBD). The biological activities of the optimized extract and the infusion were compared. The optimized extract was obtained using a solvent/root powder ratio of 4, 60% ethanol concentration, and 60% ultrasonic power. The optimized extract showed higher biological activities than the infusion. The optimized extract contained 16.6 mg mL-1 resveratrol, high antioxidant activities (135.1 µg TE mL-1 for DPPH, and 230.4 µg TE mL-1 for ABTS+), TPC (33.2 mg GAE mL-1), and extraction yield of 12.4%. The EC50 value (effective concentration 50) of the optimized extract was 0.194 µg mL-1, which revealed high cytotoxic activity against the Caco-2 cell line. The optimized extract could be used to develop functional beverages with high antioxidant capacity, antioxidants for edible oils, functional foods, and cosmetics.

Unraveling the relationship between conditions of ultrasonic-assisted extraction of chia mucilage and viscosity.

BACKGROUND: The application of chia mucilage still remains restricted due to the difficulty in achieving high extraction yields. The effect of ultrasonic-assisted extraction (UAE) conditions (temperature, seed:water ratio and time) on the rheological properties of chia mucilage extracts and the relation to the proportion of translucent phase (TP) and opaque phase (OP) of the mucilage in the extract were evaluated. RESULTS: UAE allowed the efficient extraction of chia mucilage from chia seeds. The desired overall optimal combination to maximize both yield and apparent viscosity was achieved at a seed:water ratio 1:10, a temperature of 25.3 °C and 53.7 min extraction time; the optimal conditions to obtain the maximum yield and minimum apparent viscosity were a seed:water ratio close to 1:20, temperature of 48.8 °C and 208.4 min extraction time. CONCLUSION: The results obtained in the present work demonstrated that the differences in rheological properties of chia mucilage extracts are due to the extraction methods used. Therefore, it is possible to modulate the extraction conditions in order to obtain different characteristics of the mucilage, maintaining a high extraction yield. © 2022 Society of Chemical Industry.

Antioxidant Capacity and Antiplatelet Activity of Aqueous Extracts of Common Bean (Phaseolus vulgaris L.) Obtained with Microwave and Ultrasound Assisted Extraction.

Phaseolus vulgaris L. has beneficial effects on several chronic non-communicable diseases (e.g., cardiovascular diseases) related to oxidative stress. This redox state may influence platelet activation and aggregation; which is crucial in thrombus formation. In this work, the antiplatelet and antioxidant potential of aqueous extracts obtained by green processes, microwave-assisted extraction and ultrasound-assisted extraction, from 25 landraces of common beans were investigated. Phenol content and antioxidant potential were determined using the Folin-Ciocalteu method, total monomeric anthocyanin and ORAC assay, respectively. The antiplatelet potential of the extracts was explored by turbidimetry. Microwave extraction showed higher phenol content and antioxidant activity in most extracts. Soja landrace extract obtained by microwave-assisted extraction showed higher phenol content and antioxidant activity (893.45 ± 87.30 mg GAE/g and 35,642.85 ± 2588.88 ORAC µmolTE/g, respectively). Although most of the extracts obtained by microwave-assisted extraction showed antiplatelet activity, the extract of Hallado Aleman landrace obtained by ultrasound-assisted extraction (IC50 = 0.152 ± 0.018 mg/mL) had the highest antiplatelet potential. The extraction method, MAE and UAE, influences the biological potential of the beans, specifically the antiplatelet activity and antioxidant activity. The functional value of this legume for direct consumption by the population was evidenced, as well as its inclusion in food formulations.

Ultrasonic-assisted extraction and automated determination of catalase and lipase activities in bovine and poultry livers using a digital movie-based flow-batch analyzer.

An ultrasonic reactor (UR) was developed and coupled to a digital movie-based flow-batch analyzer (DM-FBA) for the ultrasonic-assisted extraction (UAE) and fast determination of catalase and lipase activities in bovine and poultry livers. The lab-made UR mainly consisted of a borosilicate glass container and a piezoelectric disc. The DM-FBA mainly consisted of a webcam, an ultrasonic actuator controller, a peristaltic pump, six solenoid valves, a valve driver, a mixing chamber, a magnetic stirrer, an Arduino Mega 2560, and a personal computer. This setup, named UR-DM-FBA, was controlled by custom software. Ultrasound (US) frequency, US power, sonication time, and concentration of extraction agent were optimized using the Taguchi method. Experiments at silent conditions (mechanical stirring at 1500 rpm) were carried out to evaluate extraction efficiency. Optimized parameters for the UAE of catalase were US frequency of 30 kHz, 2.0 mL of Triton X-100, sonication time of 270 s, and US power of 10.8 W. For the UAE of lipase, the optimized parameters were US frequency of 20 kHz, 0.30 mL of triethanolamine, sonication time of 270 s, and US power of 18 W. Catalase and lipase activities obtained with the UR were, on average, 1.9 × 103% and 2.0 × 103% higher than those obtained at silent conditions, respectively, which indicates that that the lab-made UR was capable of extracting these enzymes more efficiently. Determinations using the UR-DM-FBA were highly accurate (relative error ranging from -1.98% to 1.96% for bovine catalase, -0.65% to 0.76% for bovine lipase, -2.03 to 2.08% for poultry catalase, and -0.55% to 0.64% for poultry lipase) and precise (overall coefficient of variation <0.02% for bovine and poultry catalase and <0.2% for bovine and poultry lipase). Results obtained with the proposed system and reference methods were in good agreement according to the paired t-test (95% confidence level). High sampling rates (>69 h-1) and low sample/reagent consumption (<1.6 mL) were also obtained. Due to the highly efficient UAE, the proposed system can be applied for fast and accurate quantification of lipase and catalase in biological samples with low waste generation.

Latest Insights on Novel Deep Eutectic Solvents (DES) for Sustainable Extraction of Phenolic Compounds from Natural Sources.

Phenolic compounds have long been of great importance in the pharmaceutical, food, and cosmetic industries. Unfortunately, conventional extraction procedures have a high cost and are time consuming, and the solvents used can represent a safety risk for operators, consumers, and the environment. Deep eutectic solvents (DESs) are green alternatives for extraction processes, given their low or non-toxicity, biodegradability, and reusability. This review discusses the latest research (in the last two years) employing DESs for phenolic extraction, solvent components, extraction yields, extraction method characteristics, and reviewing the phenolic sources (natural products, by-products, wastes, etc.). This work also analyzes and discusses the most relevant DES-based studies for phenolic extraction from natural sources, their extraction strategies using DESs, their molecular mechanisms, and potential applications.

Micro-computed Tomographic Assessment of Supplementary Cleaning Techniques for Removing Bioceramic Sealer and Gutta-percha in Oval Canals.

INTRODUCTION: The aim of this study was to conduct a micro-computed tomographic assessment of the effectiveness of 3 supplementary cleaning techniques in reducing the residual volume of gutta-percha and a bioceramic sealer after performing endodontic retreatment procedures in teeth with oval canals. METHODS: Thirty-six mandibular premolars were instrumented with the ProTaper Next system (instruments X1-X3; Dentsply Maillefer, Ballaigues, Switzerland) and filled with gutta-percha and Bio-C Sealer (Angelus, Londrina, PR, Brazil) using the single-cone technique. The teeth were reinstrumented with the Reciproc R40 instrument (VDW, Munich, Germany) and divided into 3 groups according to the supplementary cleaning technique used (n = 12): ultrasonic-assisted irrigation (UAI), EndoActivator (Dentsply Tulsa Dental Specialties, Tulsa, OK) irrigation (EAI), or the XP-endo Finisher R system (XPR; FKG Dentaire, La Chaux-de-Fonds, Switzerland). Micro-computed tomographic imaging was used to quantify the residual volume of filling material. One-way analysis of variance complemented by the Tukey test was used to perform the statistical analysis (P < .05). RESULTS: Significant reductions were obtained in the residual filling material after supplementary cleaning (P < .05). XPR (47.5%) led to significantly greater (P < .05) filling material removal than UAI (16.6%) or EAI (22.6%). The removal values of the 2 latter systems were not significantly different. CONCLUSIONS: XPR was more effective than UAI and EAI in removing filling material in mandibular premolars with oval canals. None of the tested supplementary cleaning techniques completely removed the residual filling material.

Analytical approaches applied to the analysis of apprehended formulations of anabolic androgenic steroids.

Anabolic androgenic steroids (AASs) comprise a class of synthetic androgens resulting from chemical modifications of testosterone, known for their illicit consumption, which can result inextensive side effects. Extraction procedures applied to the analysis of their formulations are still limited to a few methodologies, despite the increasing numbers of confiscations of AASs. In this sense, the aims of this work were to evaluate the extraction of active ingredients from formulations of anabolic agents using solid-liquid or liquid-iquid, ultrasonic bath, ultrasonicprobe, and microwave-assisted extraction. The results indicated that the extraction procedures influenced the detected concentration of AASs, as the use of ultrasonic probe and microwave irradiation increased the overall extraction of anabolic agents compared with solid-liquid, liquid-liquid, and ultrasonic bath. Regarding oxymetholone, for instance, the microwave-assisted extraction and ultrasonic probe extracted, respectively, 37.46 ± 1.36 and 35.69 ± 0.98 mg/tablet, while solid-liquid extracted 29.63 ± 0.40 mg/tablet of the activeingredient. Therefore, alternative methods such as microwave-assisted extraction or theultrasonic probe could be used for the analysis of formulations of AASs assisting with the identification of illicit and toxic components.

Phytochemicals in Garlic Extract Inhibit Therapeutic Enzyme DPP-4 and Induce Skeletal Muscle Cell Proliferation: A Possible Mechanism of Action to Benefit the Treatment of Diabetes Mellitus.

Diabetes mellitus is a severe health problem in Mexico, and its prevalence is increasing exponentially every year. Recently, DPP-4 (dipeptidyl peptidase-4) inhibitors have become attractive oral anti-hyperglycemic agents to reduce the pathology of diabetes. Gliptin's family, such as sitagliptin, vildagliptin, and alogliptin, are in clinical use to treat diabetes mellitus but possess side effects. Therefore, there is a specific need to look for new therapeutic scaffolds (biomolecules). Garlic bulb is widely used as a traditional remedy for the treatment of diabetes. The garlic extracts are scientifically proven to control glucose levels in patients with diabetes, despite the unknown mechanism of action. The aim of the study is to investigate the antidiabetic effects of ultrasonication assisted garlic bulb extract. To achieve this, in-vitro assays such as DPP-4 inhibitory and antioxidant activities were investigated. Further, functional group analysis using FTIR and identification of phytochemicals using mass spectrometry analysis was performed. The results showed that 70.9 µg/mL of garlic bulb extract inhibited 50% DPP-4 activity. On top of that, the garlic extract exhibited a 20% scavenging activity, equivalent to 10 µg/mL of ascorbic acid. Molecular docking simulations on identified phytochemicals using mass spectrometry revealed their potential binding at the DPP-4 druggable region, and therefore the possible DPP-4 inhibition mechanism. These results suggest that prepared garlic extract contains phytochemicals that inhibit DPP-4 and have antioxidant activity. Also, the prepared extract induces skeletal muscle cell proliferation that demonstrates the antidiabetic effect and its possible mechanism of action.

Ionic liquid associated with ultrasonic-assisted extraction: A new approach to obtain carotenoids from orange peel.

The aim of this study was to develop a new method for carotenoid extraction from orange peel, using ionic liquid (IL) to replace conventional organic solvents, assisted by ultrasound. Four different IL were tested: 1-butyl-3-methylimidazolium chloride ([BMIM][Cl]), 1-n-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF6]), 1-n-butyl-3-methylimidazolium tetrafluoroborate ([BMIM][BF4]), and 1-hexyl-3-methylimidazolium chloride ([HMIM][Cl]). Response surface methodology was applied in order to optimize the carotenoid extraction conditions, and Amberlite XAD-7HP resin was used to separate the carotenoids from the IL, allowing their recovery. Determination of carotenoids was carried out by high-performance liquid chromatography coupled to photodiode array and mass spectrometry detectors (HPLC-DAD-MSn). Thermal stability at different temperatures (60 °C and 90 °C) and peroxyl radical scavenging activity of the carotenoid extracts obtained with acetone and IL were evaluated. [BMIM][Cl] was the most effective IL, leading to a total carotenoid content of 32.08 ±â€¯2.05 µg/g, while 7.88 ±â€¯0.59 µg/g of dry matter was obtained by acetone extraction. IL and carotenoid recoveries using XAD-7HP resin were in the range of 59.5-63.8% and 52.2-58.7%, respectively. A carotenoid extract was successfully obtained with IL, finally isolated just by using ethanol, besides being more stable and presenting higher antioxidant activity than that obtained with acetone.

UPLC-ESI-QTOF-MS²-Based Identification and Antioxidant Activity Assessment of Phenolic Compounds from Red Corn Cob (Zea mays L.).

In this study, the extraction of phenolic antioxidants from red corn cob was carried out using ultrasound-assisted extraction (UAE). The solid:liquid ratio and extraction time were evaluated when obtaining these bioactive compounds. The total phenolic contents were evaluated using the Folin Ciocalteu method, while the antioxidant activity was measured by ABTS•+ and DPPH• assays. The amount of phenolic compounds ranged from 215.17 ± 33.49 to 527.33 ± 103.79 GAE mg/100 g and, overall, high solid:liquid ratios and time periods release more phenolic compounds. Moreover, the red corn cob extracts showed higher radical scavenging capacity according to the results obtained using the ABTS•+ technique compared to the DPPH• test. The coupling of liquid chromatography and mass spectrometry assay allowed the determination of 11 phenolic compounds, including phenolic acids and flavonoids. Thus, our results demonstrated for the first time the potential of red corn cob as a source of bioactive compounds, which might be included in food and pharmacological preparations.

Ultrasonic-assisted extraction combined with sample preparation and analysis using LC-ESI-MS/MS allowed the identification of 24 new phenolic compounds in pecan nut shell [Carya illinoinensis (Wangenh) C. Koch] extracts.

Ultrasonic-assisted extraction combined with statistical tools (factorial design, response surface methodology and kinetics) were used to evaluate the effects of the experimental conditions of temperature, solid-to-solvent ratio, ethanol concentration and time for the extraction of the total phenolic content from pecan nut shells. The optimal conditions for the aqueous and hydroalcoholic extract (with 20% v/v of ethanol) were 60 and 80 °C; solid to solvent ratio of 30 mL·g-1 (for both) and extraction time of 35 and 25 min, respectively. Using these optimize extraction conditions, 426 and 582 mg GAE·g-1 of phenolic compounds, from the aqueous and hydroalcoholic phases respectively, were obtained. In addition, the analysis of the phenolic compounds using the LC-ESI-MS/MS system allowed the identification of 29 phenolic compounds, 24 of which had not been reported in literature for this raw material yet.