Optimization of Ultrasound-Assisted Extraction and Characterization of the Phenolic Compounds in Rose Distillation Side Streams Using Spectrophotometric Assays and High-Throughput Analytical Techniques.

Lately, the essential oils industry has been one of the most expanding markets globally. However, the byproducts generated after the distillation of aromatic plants and their transformation to novel high-added value products consist of a major up-to-date challenge. Thus, the scope of the current study is the optimization of ultrasound-assisted extraction (UAE) for the recovery of phenolic compounds from rose (Rosa damascena) post-distillation side streams using Box-Behnken design. In particular, the highest total phenolic content (TPC) was achieved at 71% v/v ethanol-water solution, at 25 min, 40 mL/g dry sample and 53% ultrasound power, while ethanol content and extraction time were the most crucial factors (p-value ≤ 0.05) for UAE. Both solid (RSB) and liquid (LSB) rose side streams exhibited significant antiradical and antioxidant activities. The interpretation of attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectra confirmed the presence of compounds with properties such as phenolic compounds, phenolic amide derivatives, and alcohols in the extracts. Moreover, the flavonoids naringenin, quercetin, and kaempferol were the major phenolic compounds, identified in the extracts by liquid chromatography-tandem mass spectrometry analysis (LC-MS/MS), followed by gallic, protocatechuic, p-hydroxybenzoic, and rosmarinic acids. Furthermore, the LC-MS/MS results pinpointed the effect of factors other than the extraction conditions (harvesting parameters, climatic conditions, plant growth stage, etc.) on the phenolic fingerprint of RSB extracts. Therefore, RSB extracts emerge as a promising alternative antioxidant agent in food products.

Optimization of Ultrasound- and Microwave-Assisted Extraction for the Determination of Phenolic Compounds in Peach Byproducts Using Experimental Design and Liquid Chromatography-Tandem Mass Spectrometry.

The conversion of plant byproducts, which are phenolic-rich substrates, to valuable co-products by implementing non-conventional extraction techniques is the need of the hour. In the current study, ultrasound- (UAE) and microwave-assisted extraction (MAE) were applied for the recovery of polyphenols from peach byproducts. Two-level screening and Box-Behnken design were adopted to optimize extraction efficiency in terms of total phenolic content (TPC). Methanol:water 4:1% v/v was the extraction solvent. The optimal conditions of UAE were 15 min, 8 s ON-5 s OFF, and 35 mL g-1, while MAE was maximized at 20 min, 58 °C, and 16 mL g-1. Regarding the extracts' TPC and antioxidant activity, MAE emerged as the method of choice, whilst their antiradical activity was similar in both techniques. Furthermore, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to determine chlorogenic acid and naringenin in byproducts' extracts. 4-Chloro-4'-hydroxybenzophenone is proposed as a new internal standard in LC-MS/MS analysis in foods and byproducts. Chlorogenic acid was extracted in higher yields when UAE was used, while MAE favored the extraction of the flavonoid compound, naringenin. To conclude, non-conventional extraction could be considered as an efficient and fast alternative for the recovery of bioactive compounds from plant matrices.

Effects of Non-Polar Dietary and Endogenous Lipids on Gut Microbiota Alterations: The Role of Lipidomics.

Advances in sequencing technologies over the past 15 years have led to a substantially greater appreciation of the importance of the gut microbiome to the health of the host. Recent outcomes indicate that aspects of nutrition, especially lipids (exogenous or endogenous), can influence the gut microbiota composition and consequently, play an important role in the metabolic health of the host. Thus, there is an increasing interest in applying holistic analytical approaches, such as lipidomics, metabolomics, (meta)transcriptomics, (meta)genomics, and (meta)proteomics, to thoroughly study the gut microbiota and any possible interplay with nutritional or endogenous components. This review firstly summarizes the general background regarding the interactions between important non-polar dietary (i.e., sterols, fat-soluble vitamins, and carotenoids) or amphoteric endogenous (i.e., eicosanoids, endocannabinoids-eCBs, and specialized pro-resolving mediators-SPMs) lipids and gut microbiota. In the second stage, through the evaluation of a vast number of dietary clinical interventions, a comprehensive effort is made to highlight the role of the above lipid categories on gut microbiota and vice versa. In addition, the present status of lipidomics in current clinical interventions as well as their strengths and limitations are also presented. Indisputably, dietary lipids and most phytochemicals, such as sterols and carotenoids, can play an important role on the development of medical foods or nutraceuticals, as they exert prebiotic-like effects. On the other hand, endogenous lipids can be considered either prognostic indicators of symbiosis or dysbiosis or even play a role as specialized mediators through dietary interventions, which seem to be regulated by gut microbiota.

Towards the Optimization of Microwave-Assisted Extraction and the Assessment of Chemical Profile, Antioxidant and Antimicrobial Activity of Wine Lees Extracts.

Wine lees, a sub-exploited byproduct of vinification, is considered a rich source of bioactive compounds, such as (poly)phenols, anthocyanins and tannins. Thus, the effective and rapid recovery of these biomolecules and the assessment of the bioactive properties of wine lees extracts is of utmost importance. Towards this direction, microwave-assisted extraction (MAE) factors (i.e., extraction time, microwave power and solvent/material ratio) were optimized using experimental design models in order to maximize the (poly)phenolic yield of the extracts. After optimizing the MAE process, the total phenolic content (TPC) as well as the antiradical, antioxidant and antimicrobial activity of the extracts were evaluated. Furthermore, Fourier transform infrared spectroscopy (FTIR) was employed to investigate the chemical profile of wine lees extracts. Red varieties exhibited higher biological activity than white varieties. The geographical origin and fermentation stage were also considered as critical factors. The white variety Moschofilero presented the highest antioxidant, antiradical and antimicrobial activity, while Merlot and Agiorgitiko samples showed noteworthy activities among red varieties. Moreover, IR spectra confirmed the presence of sugars, amino acids, organic acids and aromatic compounds. Thus, an efficient, rapid and eco-friendly process was proposed for further valorization of wine lees extracts.

Antioxidant Profiles of Vitis vinifera L. and Salvia triloba L. Leaves Using High-Energy Extraction Methodologies.

The profiles of Vitis vinifera L. and Salvia triloba L. leaf extracts have been studied via photometric assays on the basis of their total phenolic and flavonoid content as well as of their radical scavenging and antioxidant activities. Ultrasound-assisted (UAE) and pressurized liquid extractions (PLE) were implemented for producing polar fractions from the plants, using different methanol-water and glycerol-water mixtures for UAE and PLE, respectively. Aqueous methanol was proved an effective solvent for the UAE of total phenolics and flavonoids as well as for increased radical scavenging and antioxidant activities. As for PLE, plain water was proved a more efficient solvent than hydroglycerolic mixtures. Overall, irrespective of the solvent(s) used, UAE extracts showed higher values compared with the PLE extracts for all the photometric determinations and for both plant species. Moreover, Salvia UAE and PLE extracts presented higher total phenolic and flavonoid contents, accompanied by higher radical scavenging and antioxidant activities, compared with Vitis extracts. The correlations among photometric results were also studied, indicating the categories of compounds that relate to the antioxidant and/or radical scavenging activities of the extracts. Mixtures of the examined extracts could be exploited as the basis of novel phytotherapeutic products in the cosmetic sector.

Macular carotenoids in lipid food matrices: DOE-based high energy extraction of egg yolk xanthophylls and quantification through a validated APCI(+) LC-MS/MS method.

Lutein and zeaxanthin exhibit significant biological activities therefore their dietary intake through carotenoid-rich foods and supplements is strongly recommended as preventive approach. Hence their extraction from natural substrates targets to their commercial exploitation as nutraceuticals and ocular pharmaceuticals. Since carotenoids' bioavailability is higher in fat-containing substrates, egg yolk is considered an ideal food matrix. DOE-based optimization of novel high energy extraction practices achieves efficient recovery of xanthophylls from lipid sources. In this research, 23 full factorial and Box-Behnken designs (BBD) were applied for optimizing ultrasound- (UAE) and microwave-assisted extraction (MAE) variables (i.e. extraction solvent, temperature, time, US or MW power and solvent/material ratio). LC-MS/MS results pointed out the precedence of UAE in lutein and zeaxanthin extraction, where higher yields were obtained with 1:1 n-hexane-acetone as solvent mixture at 19 min, 600 W and 35 mL g-1. UAE carotenoid content was higher than MAE due to the different mechanisms laying behind the two processes and due to more complete granule rupture caused by higher US power. Evaluating the current results, DOE-based UAE analytical methodology stands out as an auspicious and sustainable alternative for commercial-based extraction of lipidic bioactive compounds for food and drug industrial applications.

Metabolic and antioxidant profiles of herbal infusions and decoctions.

This study implements NMR metabolomics and spectrophotometric studies (Folin-Ciocalteu, FRAP, ABTS) to infusions and decoctions of ten plant species in order to assess and compare the metabolic and antioxidant profiles for each botanical family. Multivariate and univariate data analyses highlighted the differences among the samples and pinpointed specific classes of compounds for each plant species as well as infusions and decoctions. The identified phenolic compounds by NMR, as well as the antioxidant profile, framed a trend of increased values in infusions compared to the decoctions. Moreover, the infusion procedure positively affected the extractability of the phenolic compounds compared to decoctions. The highest total phenolic content was found in Mentha spicata, while the lowest in Matricaria chamomilla preparations, irrespective of the preparation method. The preparation time for the decoctions was examined showing that the 15min preparations were generally found richer in phenolics and of higher antioxidant capacity.

Response surface methodology toward the optimization of high-energy carotenoid extraction from Aristeus antennatus shrimp.

High-energy assisted extraction techniques, like ultrasound assisted extraction (UAE) and microwave assisted extraction (MAE), are widely applied over the last years for the recovery of bioactive compounds such as carotenoids, antioxidants and phenols from foods, animals and herbal natural sources. Especially for the case of xanthophylls, the main carotenoid group of crustaceans, they can be extracted in a rapid and quantitative way with the use of UAE and MAE. Response surface methodology (RSM) is used for the optimization of extraction methodologies, also being applied to optimize high energy techniques. Three independent variables, namely extraction time, ultrasound or microwave power and solvent/material ratio, were investigated for both methods by employing a 16-run three-level Box-Behnken design (BBD). Considering the extraction efficiency for carotenoids from Aristeus antennatus shrimp, the selected conditions for UAE were 5 min, 600 W and 10:1 mL g(-1). Acetone was the solvent of choice for the extraction procedure. For MAE, the best experimental values were 7 min, 30 W and 20:1 mL g(-1) using n-hexane:acetone:ethanol 2:1:1 (v/v/v) as extraction solvent. The determination of total carotenoid yield was carried out using the spectophotometric calibration curve (A=0.1646(±0.0061)C-0.005(±0.022), R(2)=0.996, n=3) of a standard mix solution of canthaxanthin, zeaxanthin and lutein at 452.1 nm. Under the selected conditions, the yield of total carotenoids for UAE was 23.4(±2.3) and 6.73(±0.56) mg of carotenoids per 100 g dry sample for the head and the body of shrimp, while for MAE was 23.92(±0.63) and 13.3(±1.1) mg of carotenoids per 100g dry sample, respectively. The recovery of both methods was calculated between 60 and 105%. The results indicate that high-energy extraction techniques are faster, less laborious, more repeatable and reproducible methods than the conventional approaches for the quantitative recovery of sensitive bioactive compounds. Moreover, the recovery of a high-added value group of bioactive molecules from natural sources, such as carotenoids, can constitute a profitable and valuable commercial alternative, as these compounds can be used as dietary supplements, food color enhancers and additives in animal feeds, functional foods, preservatives, pharmaceuticals and cosmetics.