Optimization of Pressurized Liquid Extraction (PLE) Parameters for Extraction of Bioactive Compounds from Moringa oleifera Leaves and Bioactivity Assessment.

Moringa oleifera leaves are rich sources of bioactive compounds with potential health benefits, including antioxidants and anti-inflammatory agents. Pressurized liquid extraction (PLE) stands out as a promising technique for effectively extracting valuable compounds from natural sources. In this study, we aimed to optimize PLE parameters, such as temperature, extraction duration, and pressure, to maximize bioactive compound (polyphenols, flavonoids, and ascorbic acid) yield from M. oleifera leaves and evaluate their antioxidant and anti-inflammatory activities. According to the outcomes of this research, the maximum achieved total polyphenol content was 24.10 mg gallic acid equivalents (GAE)/g of dry weight (dw), and the total flavonoid content was increased up to 19.89 mg rutin equivalents (RtE)/g dw. Moreover, after HPLC-DAD analysis, neochlorogenic and chlorogenic acids, catechin and epicatechin, rutin, and narirutin were identified and quantified. As far as the optimum ascorbic acid content is concerned, it was found to be 4.77 mg/g dw. The antioxidant activity was evaluated by three different methods: ferric reducing antioxidant power (FRAP), the DPPH method, and the anti-hydrogen peroxide activity (AHPA) method, resulting in 124.29 µmol ascorbic acid equivalent (AAE)/g dw, 131.28 µmol AAE/g dw, and 229.38 µmol AAE/g dw values, respectively. Lastly, the albumin denaturation inhibition was found to be 37.54%. These findings underscore the potential of PLE as an efficient extraction method for preparing extracts from M. oleifera leaves with the maximum content of bioactive compounds.

Organosolv Treatment of Red Grape Pomace for Effective Recovery of Antioxidant Polyphenols and Pigments Using a Ternary Glycerol/Ethanol/Water System under Mild Acidic Conditions.

The purpose of this investigation was (i) the development of a novel, green tertiary solvent system, composed of water, ethanol and glycerol, and (ii) the implementation of an organosolv treatment of red grape pomace (RGP) for the efficient production of polyphenol-containing extracts with enhanced antioxidant properties. The treatment developed was performed under mild acidic conditions, imparted by the addition of citric acid, and it was first evaluated on the basis of severity, establishing linear models that described the correlation between treatment performance and combined severity factors. To solicit treatment optimization, response surface methodology was implemented, considering solvent acidity and residence time as the treatment variables. The optimized treatment afforded maximum total polyphenol (166 ± 6 mg GAE g-1 DM), total pigment (4.4 ± 0.2 mg MvE g-1 DM) and total flavanol (31.5 mg CtE g-1 DM) yields and extracts with particularly enhanced antioxidant activity. This might be attributed to specific constituents with high antioxidant potency, such as catechin, determined in the extract using high-performance liquid chromatography. Thus, the treatment developed is proposed as a highly efficient process to generate RGP extracts enriched in polyphenolic compounds, with enhanced antioxidant activity. Such extracts might then be valorized as food additives, to provide antioxidant protection and/or pigmentation.

Polyphenol Extraction from Food (by) Products by Pulsed Electric Field: A Review.

Nowadays, more and more researchers engage in studies regarding the extraction of bioactive compounds from natural sources. To this end, plenty of studies have been published on this topic, with the interest in the field growing exponentially. One major aim of such studies is to maximize the extraction yield and, simultaneously, to use procedures that adhere to the principles of green chemistry, as much as possible. It was not until recently that pulsed electric field (PEF) technology has been put to good use to achieve this goal. This new technique exhibits many advantages, compared to other techniques, and they have successfully been reaped for the production of extracts with enhanced concentrations in bioactive compounds. In this advancing field of research, a good understanding of the existing literature is mandatory to develop more advanced concepts in the future. The aim of this review is to provide a thorough discussion of the most important applications of PEF for the enhancement of polyphenols extraction from fresh food products and by-products, as well as to discuss the current limitations and the prospects of the field.

Response Surface Optimization for the Enhancement of the Extraction of Bioactive Compounds from Citrus limon Peel.

Citrus limon is among the species of the genus Citrus that dominates the world market. It is highly nutritious for humans as it contains twice the amount of the suggested daily intake of ascorbic acid and is also a good source of phenolic compounds, carotenoids, and other bioactive compounds. This study aimed to identify the optimal extraction procedures and parameters to obtain the maximum quantity of bioactive components from lemon peel by-products. Various extraction techniques, including stirring, ultrasound, and pulsed electric field, were evaluated, along with factors such as extraction time, temperature, and solvent composition. The results revealed that simple stirring for 150 min at 20 °C proved to be the most effective and practical method. The ideal solvent mixture consisted of 75% ethanol and 25% water, highlighting the crucial role of solvent composition in maximizing extraction efficiency. Among the extracted compounds were phenolics, ascorbic acid, and carotenoids. Under optimum extraction conditions, the extract was found to contain high total phenolic content (TPC) (51.2 mg of gallic acid equivalents, GAE/g dry weight), total flavonoid content (TFC) (7.1 mg of rutin equivalents, RtE/g dry weight), amounts of ascorbic acid (3.7 mg/g dry weight), and total carotenoids content (TCC) (64.9 µg of ß-carotene equivalents, CtE/g). Notably, the extracts demonstrated potent antioxidant properties (128.9 µmol of ascorbic acid equivalents, AAE/g; and 30.3 µmol of AAE/g as evidenced by FRAP and DPPH assays, respectively), making it a promising ingredient for functional foods and cosmetics. The study's implications lie in promoting sustainable practices by converting lemon peel into valuable resources and supporting human health and wellness through the consumption of natural antioxidants.

Optimization of Extraction Parameters for Enhanced Recovery of Bioactive Compounds from Quince Peels Using Response Surface Methodology.

Quinces are well known for their multiple health benefits, including antioxidant, hypoglycemic, antimicrobial, anti-inflammatory, anticarcinogenic, etc., properties. Despite the widespread utilization of various plant parts, the peel has been largely ignored in the industry. In this study, we explored the effects of different extraction parameters, such as temperature, time, and composition of the extraction solvent, and techniques such as ultrasound (US) and a pulsed electric field (PEF), either alone or in combination, and optimized these parameters using a response surface methodology (RSM) to enhance the extraction of bioactive compounds such as chlorogenic acid, total polyphenols, flavonoids, and ascorbic acid from waste quince peels. From our results, it was apparent that quince peels are a great source of many bioactive compounds with high antioxidant activity. More specifically, after principal component analysis (PCA) and partial least squares (PLS) analysis, quince peels contain high levels of total polyphenols (43.99 mg gallic acid equivalents/g dw), total flavonoids (3.86 mg rutin equivalents/g dw), chlorogenic acid (2.12 mg/g dw), and ascorbic acid (543.93 mg/100 g dw), as well as antioxidant activity of 627.73 µmol AAE/g and 699.61 µmol DPPH/g as evidenced by FRAP and DPPH assays, respectively. These results emphasize the potential of utilizing quince peels as an eco-friendly and cost-effective source of bioactive compounds with various applications in the food and pharmaceutical industries for the prepared extracts.

Determination of the Total Phenolics Content and Antioxidant Activity of Extracts from Parts of Plants from the Greek Island of Crete.

Oxidative damages are responsible for many adverse health effects and food deterioration. The use of antioxidant substances is well renowned, and as such, much emphasis is placed on their use. Since synthetic antioxidants exhibit potential adverse effects, plant-derived antioxidants are a preferable solution. Despite the myriads of plants that exist and the fact that numerous studies have been carried out so far, there are many species that have not been examined so far. Many plants under research exist in Greece. Trying to fill this research gap, the total phenolics content and antioxidant activity of seventy methanolic extracts from parts of Greek plants were evaluated. The total phenolics content was measured by the Folin-Ciocalteau assay. Their antioxidant capacity was calculated by the 2,2-Diphenyl-1-picrylhydrazyl (DPPH) scavenging test, the Rancimat method based on conductometric measurements, and the thermoanalytical method DSC (Differential Scanning Calorimetry). The tested samples were obtained from several parts of fifty-seven Greek plant species belonging to twenty-three different families. Both a remarkably high phenolic content (with gallic acid equivalents varying between 311.6 and 735.5 mg/g of extract) and radical scavenging activity (IC50 values ranged from 7.2 to 39.0 µg/mL) were found in the extract of the aerial parts of Cistus species (C. creticus subsp. creticus, C. creticus subsp. eriocephalus, C. monspeliensis, C. parviflorus and C. salviifolius), Cytinus taxa (C. hypocistis subsp. hypocistis, C. hypocistis subsp. orientalis and C. ruber), and Sarcopoterium spinosum. Furthermore, the sample of Cytinus ruber showed the highest protection factor (PF = 1.276) regarding the Rancimat method, which was similar to that of butylated hydroxytoluene (BHT) (PF = 1.320). The results indicated that these plants are rich in antioxidant compounds, potentiating their use either as food additives to enhance the antioxidant properties of food products, or protect them from oxidation, or as sources for the preparation of food supplements with antioxidant properties.

Waste Orange Peels as a Feed Additive for the Enhancement of the Nutritional Value of Tenebrio molitor.

Lately, additional attention is being placed on edible insects, since they constitute an excellent, cost-efficient source of proteins with a low ecological footprint. Tenebrio molitor was the first insect that was considered edible by EFSA in 2021. This species can replace conventional protein sources and thus, it has the potential to be used in many different food products. In the present study, a food by-product that is commonly produced (i.e., albedo orange peel waste) was used as a feed additive for T. molitor larvae, in an effort to further improve the circular economy and enhance the nutritional value of the insects. To this end, bran, which is commonly used as feed for T. molitor larvae, was fortified with the albedo orange peel waste (up to 25% w/w). Larval performance, in terms of larval survival and growth, as well as the larval nutritional value, i.e., the content of protein, fat, carbohydrates, ash, carotenoids, vitamins A and C, and polyphenols, was evaluated. Based on the results, the increase in the percentage of orange peel albedos in T. molitor feed resulted in a subsequent increase in the content of larvae in carotenoids and vitamin A up to 198%, in vitamin C up to 46%, and an increase in the protein and ash content up to 32% and 26.5%, respectively. Therefore, the use of albedo orange peel waste for feeding of T. molitor larvae is highly recommended, since it results in larvae with enhanced nutritional value and at the same time, the utilization of this feeding substrate further lowers the cost of insect farming.

Evaluation of the Efficacy and Synergistic Effect of α- and δ-Tocopherol as Natural Antioxidants in the Stabilization of Sunflower Oil and Olive Pomace Oil during Storage Conditions.

Tocopherols are natural bioactive compounds with several health benefits. This study evaluated the effect of different ratios of α- and δ- tocopherol homologs to protect sunflower oil (SO) and olive pomace oil (OPO) against oxidation. A synergistic effect was recorded when the two tocopherols were combined at a ratio of 7:1 (α-T/δ-T). The oil samples were exposed to accelerated oxidation conditions using a Rancimat (90 °C and airflow of 15 L/h for 24 h) and protection from tocopherols was compared with that from butylated hydroxytoluene (BHT). Assessment of oil stability was examined using well-known parameters such as peroxide value (PV), thiobarbituric acid reactive substances (TBARS), p-anisidine value (p-AV), conjugated dienes (CD) and trienes (CT), and total oxidation (Totox) value, which were all significantly reduced when tocopherols were added at a ratio of 7:1 α-T/δ-T. Primary oxidative compounds measured according to PV were only reduced in SO samples (6.11%). Off-flavor compounds measured via TBARS assay in SO samples were reduced by above 20%, while p-AV was also reduced. CDvalue was correlated with PV in SO samples, while the 7:1 mixture was more effective than BHT for CTvalue. Total oxidation values in SO samples and OPO samples were reduced by 6.02% and 12.62%, respectively. These values in SO samples also provided a remarkable correlation (R2 > 0.95) with incubation time. Moreover, the synergistic effect was not only effective in reducing the oxidation values of oil samples, but also in lowering the degradation rate of tocopherols. Protective effects from tocopherols were mainly observed in SO samples, as OPO samples were more resistant to oxidation processes. This effect was even observed in fatty acid analysis, where the 7:1 mixture provided better results than BHT-spiked samples. Thus, it is suggested that tocopherol mixtures might be used as a natural preservative in the food industry to restrain lipid oxidation processes.

Untargeted metabolomics of human keratinocytes reveals the impact of exposure to 2,6-dichloro-1,4-benzoquinone and 2,6-dichloro-3-hydroxy-1,4-benzoquinone as emerging disinfection by-products.

INTRODUCTION: The 2,6-dichloro-1,4-benzoquinone (DCBQ) and its derivative 2,6-dichloro-3-hydroxy-1,4-benzoquinone (DCBQ-OH) are disinfection by-products (DBPs) and emerging pollutants in the environment. They are considered to be of particular importance as they have a high potential of toxicity and they are likely to be carcinogenic. OBJECTIVES: In this study, human epidermal keratinocyte cells (HaCaT) were exposed to the DCBQ and its derivative DCBQ-OH, at concentrations equivalent to their IC20 and IC50, and a study of the metabolic phenotype of cells was performed. METHODS: The perturbations induced in cellular metabolites and their relative content were screened and evaluated through a metabolomic study, using 1H-NMR and MS spectroscopy. RESULTS: Changes in the metabolic pathways of HaCaT at concentrations corresponding to IC20 and IC50 of DCBQ-OH involved the activation of cell membrane α-linolenic acid, biotin, and glutathione and deactivation of glycolysis/gluconeogenesis at IC50. The changes in metabolic pathways at IC20 and IC50 of DCBQ were associated with the activation of inositol phosphate, pertaining to the transfer of messages from the receptors of the membrane to the interior as well as with riboflavin. Deactivation of biotin metabolism was recorded, among others. The cells exposed to DCBQ exhibited a concentration-dependent decrease in saccharide concentrations. The concentration of steroids increased when cells were exposed to IC20 and decreased at IC50. Although both chemical factors stressed the cells, DCBQ led to the activation of transporting messages through phosphorylated derivatives of inositol. CONCLUSION: Our findings provided insights into the impact of the two DBPs on human keratinocytes. Both chemical factors induced energy production perturbations, oxidative stress, and membrane damage.

Melamine sponge functionalized with carbon nanodots for the extraction of polyaromatic hydrocarbons and musks from environmental samples prior to their determination by gas chromatography-mass spectrometry.

In this study, the functionalization of melamine sponge (MeS) with graphene quantum dots (GQDs) and its use as a sorbent for the extraction of polycyclic aromatic hydrocarbons (PAHs) and musks from environmental samples are presented. The MeS@GQDs is prepared by modification of the MeS with GQDs in a one-pot, single-step, in situ synthesis, using citric acid as carbon source. The produced MeS@GQDs was used to develop and optimize an analytical method based on solid-phase extraction mode, for the subsequent analysis of soil samples and treated effluents exploiting the extraction properties of the synthesized MeS@GQDs. The developed method not only presented satisfactory repeatability (RSD<8.7%) and inter-day repeatability (RSD<9.6%), but also its limits of quantification were found to be low (15-80 ng L-1). Moreover, the proposed method was linear in a wide range of concentrations (0.015-11.8 µg L-1) and the recoveries from difficult matrixes, such as treated effluents and soil, were satisfactory. Overall, the use of the sorbent for the development of a new analytical method was found to be advantageous as compared with other reported methods.

Olive Oil Produced from Olives Stored under CO2 Atmosphere: Volatile and Physicochemical Characterization.

In this study, an alternative debittering technique for olives, invented and patented by Prof. Vassilis Dourtoglou, was employed. Olive fruits (Olea europaea cv. Megaritiki) were stored under CO2 atmosphere immediately after harvest for a period of 15 days. After the treatment, a sensory evaluation between the olives stored under CO2 and those stored under regular atmospheric conditions (control) was performed. Additionally, the CO2-treated olives were used for the cold press of olive oil production. The volatile profile of the olive oil produced was analyzed using headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to mass spectrometry (GC-MS). A total of thirty different volatile compounds were detected. The volatile characteristics of olive oil are attributed, among others, to aldehydes, alcohols, esters, hydrocarbons, alkanes, and terpenes. The volatile compounds' analysis showed many differences between the two treatments. In order to compare the volatile profile, commercial olive oil was also used (produced from olives from the same olive grove with a conventional process in an industrial olive mill). The antioxidant activity, the content of bioactive compounds (polyphenols, α-tocopherol, carotenoids, and chlorophylls), and the fatty acids' profile were also determined. The results showed that the oil produced from CO2-treated olives contains different volatile components, which bestow a unique flavor and aroma to the oil. Moreover, this oil was found comparable to extra virgin olive oil, according to its physicochemical characteristics. Finally, the enhanced content in antioxidant compounds (i.e., polyphenols) not only rendered the oil more stable against oxidation but also better for human health. The overall quality of the olive oil was enhanced and, as such, this procedure holds great promise for future developments.

Matrix solid-phase dispersion based on magnetic ionic liquids: An alternative sample preparation approach for the extraction of pesticides from vegetables.

In this study, we propose, for the first time, the direct use of a magnetic ionic liquid (MIL) in a matrix solid-phase extraction procedure. Because of the magnetic properties, the MIL can be harvested directly after the extraction step, using a magnet, while its hydrophobic nature makes feasible the extraction of analytes. Raw vegetables of high water content can be analyzed without any pretreatment. The viscous nature of the selected MIL assists in blending with the matrix, while its hydrophobicity facilitates easier separation and retrieval. Additionally, no solid dispersing materials or co-sorbents are needed. A simple, low-cost analytical method for the determination of multi-class pesticides residues in raw vegetables was developed, with satisfactory recoveries.

Melamine Sponge Functionalized with Urea-Formaldehyde Co-Oligomers as a Sorbent for the Solid-Phase Extraction of Hydrophobic Analytes.

A new procedure for the functionalization of melamine sponge (MeS) with urea-formaldehyde (UF) co-oligomers is put forward. The procedure differs from the typical synthesis of the UF co-polymer, as it employs a base-catalyzed condensation step at certain concentrations of urea and formaldehyde. The produced melamine-urea-formaldehyde (MUF) sponge cubes are hydrophobic, despite the presence of hydrophilic groups in the oligomers. The MUF sponge developed herein is used as a sorbent for the solid-phase extraction of 10 analytes, from 6 different classes (i.e., non-steroidal anti-inflammatory drugs, benzophenones, parabens, phenols, pesticides and musks) and an analytical method is developed for their liquid chromatographic separation and detection. Low limits of quantification (0.03 and 1.0 µg L-1), wide linear ranges and excellent recoveries (92⁻100%) are some of the benefits of the proposed procedure. The study of the synthesis conditions of MUF cubes reveals that by altering them the hydrophilic/lipophilic balance of the MUF cubes can be tuned, hinting towards a strong potential for many other applications.

Two of a kind but different: Luminescent carbon quantum dots from Citrus peels for iron and tartrazine sensing and cell imaging.

Citrus sinensis and Citrus limon peels were used to synthesize two different kinds of carbon quantum dots (CQDs) via an unsophisticated and inexpensive carbonization procedure. The proposed synthesis is straightforward and adheres to the principles of green chemistry since no organic solvents are used and no toxic by-products are formed, while the residual resources employed facilitate the large scale synthesis of dots. The Citrus sinensis and Citrus limon peels are proved to be excellent precursors for the synthesis of CQDs with highly practical applications. The CQDs display strong excitation-independent, blue fluorescence, which is stable over time. Splendid water dispersibility, photostability and stability over a wide range of pH are some of the main advantages of the CQDs, which enable them to be used as a fluorescent probes. Although many of their features are alike, our findings demonstrate that each kind of the CQDs lend itself to quite distinct analytical applications. The developed fluorescent probes possess high potential for sensitive and selective detection of Fe3+ (Citrus sinensis CQDs) and tartrazine (Citrus limon CQDs) via a quenching mechanism. The decrease in fluorescence intensity is in linear relationship with the concentrations of Fe3+ and tartrazine in the ranges of 0.01-1.0µM and 0.6-23.5µΜ, respectively. Moreover, their low cytotoxicity reinforces their applicability towards cell bioimaging and intracellular detection of Fe3+, which were further studied.

Octyl-modified magnetic graphene as a sorbent for the extraction and simultaneous determination of fragrance allergens, musks, and phthalates in aqueous samples by gas chromatography with mass spectrometry.

An effective, simple, and low-cost sample preparation method based on dispersive SPE followed by GC with MS is developed for the multianalyte determination of fragrance allergens, musks, and phthalates, at sub-ppb levels. The extraction procedure is based on a novel magnetic graphene sorbent, which is functionalized with octylamine, taking advantage of the functionalization's hydrophobic properties and π-π interactions with the analytes. Two alkyl amines, the octylamine and octadecylamine are studied to introduce alkyl chains in the basal plane of graphene. Magnetic graphene- octadecylamine is proved to be highly hydrophobic to such a degree that is hard to disperse in the bulk aqueous matrixes. Because of this behavior, its extraction efficiency for the target analytes is low. The synthesis and applicability of the magnetic graphene-octylamine as more favored sorbent are optimized in terms of the most determining experimental conditions. The detection and quantification limits, which are calculated based on S/N ratio of 3 and 10, respectively, ranged from 0.29 to 3.2 ng L(-1) and from 0.89 to 9.6, respectively. The dispersive SPE is successfully applied to routine analysis for the determination of the target analytes in samples from municipal treatment plant of Ioannina (Greece), from Pamvotis Lake and baby bathwater. The reproducibility of the spiked biological treatment plant water sample is evaluated and the relative standard deviation values range between 2.1 and 9.4%.