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This study provides the first comprehensive evaluation of the bioactive potential of acorn flour extracts ( Quercus robur , Fagaceae) prepared at different temperatures (20, 60, 80 and 100 °C), focusing on polyphenolic content, antioxidant properties and enzyme inhibitory activities. Through HPLC-ESI-MS/MS analysis, 36 bioactive compounds were identified, with the extract at 60 °C showing the highest concentrations of key polyphenols, notably gallic acid (210,008.9 mg·kg -1 ) and ellagic acid (45,469.6 mg·kg -1 ). This extract also exhibited a high antioxidant activity and significant inhibition of glucosidase and acetylcholinesterase, suggesting potential benefits for diabetes management and neuroprotection. The results indicate that extraction temperature affects bioactivity, with the 60 °C extract standing out as a promising candidate for nutraceutical, pharmaceutical, and cosmeceutical applications due to its rich polyphenol profile and potent biological properties.

The present study was designed to determine the phenolic constituents, antioxidant, and enzyme inhibition activities of aerial parts and bulbs of Allium lycaonicum (family Amaryllidaceae). Extracts were prepared by maceration and Soxhlet/infusion using hexane, methanol, and water as extraction solvents. Generally, extracts from the aerial parts showed higher total phenolic and individual components and antioxidant activity than their respective bulb extracts. Maceration with water was the best to extract total phenolic content from the aerial parts (29.00 mg gallic acid equivalents (GAE)/g), while the Soxhlet extraction with hexane (22.29 mg GAE/g) was the best for the bulb. Maceration with methanol recovered the highest total flavonoid content from both the aerial parts (41.95 mg (rutin equivalents (RE)/g) and bulb (1.83 mg RE/g). Polar extracts of aerial parts were characterized by higher abundance of kaempferol-3-glucoside (≤20,624.27 µg/mg), hyperoside (≤19,722.76 µg/g), isoquercitrin (≤17,270.70 µg/g), delphindin-3,5-diglucoside (≤14,625.21 µg/g), and rutin (≤10,901.61 µg/g) than the bulb. Aerial parts' aqueous extract, prepared by maceration, exerted the highest anti-ABTS (2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) radical activity (64.09 mg trolox equivalents (TE)/g), Cu ++ (83.03 mg TE/g) and Fe +++ (63.03 mg TE/g) reducing capacity while that prepared by infusion recorded the highest anti-DPPH (2,2-diphenyl-1-picrylhydrazyl) radical (31.70 mg TE/g) and metal chelating (27.66 mg EDTAE/g) activities. The highest total antioxidant activity (1.46 mmol TE/g) was obtained by maceration of the bulb with water. Extracts obtained by organic solvents showed remarkable enzyme inhibition properties against the tested enzymes. Soxhlet extraction of the bulb with hexane and methanol recorded the highest acetylcholinesterase inhibition (4.75 mg galanthamine equivalents (GALAE)/g) and tyrosinase inhibition (139.95 mg kojic acid equivalents/g) activities, respectively. Extracts obtained by maceration of the bulb with methanol and the aerial parts with hexane exerted the highest glucosidase inhibition (3.25 mmol acarbose equivalents/g) and butyrylcholinesterase inhibition (20.99 mg GALAE/g) activities, respectively. These data indicated that A. lycaonicum is a source of bioactive molecules with potential antioxidant and enzyme inhibition properties. Nonetheless, the extracts obtained through various solvents and extraction techniques showed variations in their phytoconstituent composition and biological properties.

Sumac, Rhus coriaria L., is employed as a natural preservative in the food sector, due to its rich content of antioxidant compounds, including hydrolysable tannins, phenolic acids, anthocyanins, and flavonoids. In this work, the phytochemical characterization of sumac fruits from five Sicilian accessions was performed to evaluate their potential as a food preservative for nutraceutical exploitation. Spectrophotometric tests and HPLC-MS/MS analyses were conducted to assess and compare the antioxidant power of the water extracts produced with the five sumac accessions. Principal component analysis was also carried out to better visualize the obtained results. Flavonoids and phenolic acids, namely isoquercitrin (20,342.82 mg/kg dry extract) and gallic acid (197,489.19 mg/kg dry extract), were more abundant in fruits from the population of San Biagio Platani, while the one from Giarratana was characterized by a higher content of anthocyanins such as cyanidin-3-glucoside (20,889.81 mg/kg dry extract). These two populations can be recognized as the most suitable settings for the implementation of sumac cultivation and the development of sumac-based products, especially for food and nutraceutical purposes.

The aim of this study was to investigate the parameters affecting the extraction of positive molecules such as chlorogenic acids and antioxidants, as well as potentially carcinogenic substances such as acrylamide, in different coffee brewing methods. Three coffee varieties, each assigned a different roasting degree, were used to prepare coffee brews following eight different preparation methods. Acrylamide was quantified using the HPLC-MS/MS instrument, while chlorogenic acids and caffeine were quantified using the HPLC-DAD system. Three spectrophotometric analyses were also performed (DPPH, TFC and TPC) to evaluate antioxidant activity. The results showed that the main brewing parameters, which have the greatest influence on the final content of these compounds, were the volume of water used, more specifically the brewing ratio (coffee to water ratio), the extraction time and the particle size of the coffee powder. In addition, the variables that have the greatest impact on the discrimination of the preparation methods studied are total chlorogenic acid content, TFC, TPC, caffeine and the DPPH assay. For this reason, the recipe and infusion parameters used for each of the extraction systems are the key factors that determine the extraction of coffee components and, consequently, the quality of the cup.

The development of functional foods in the dairy sector represents a flourishing field of technological research. In this study, an Italian fresh cheese as "giuncata" was enriched with inulin, a dietary fiber, with the aim of developing a product with improved nutritional properties in terms of prebiotic action on intestinal microbiota. An inulin concentration of ~4% w / w was determined in the fresh cheese after the fortification process, enabling the claim of being a "source of dietary fiber" (inulin > 3 g/100 g) according to the European regulation. The addition of inulin has no effect on the pH of cheese and does not relevantly influence its color as well as the total fat content (fat reduction ~0.61%) in comparison to the control. Mechanical properties of the cheese were also not markedly affected as evidenced from rheological and tensile testing analyses. Indeed, the incorporation of inulin in "giuncata" only exerts a slight "softening effect" resulting in a slightly lower consistency and mechanical resistance in comparison to the control. Overall, this study demonstrates the feasibility of producing a fiber-enriched dairy functional food from a large consumed fresh and soft cheese as "giuncata".

An untargeted gas chromatography-mass spectrometry (GC-MS) approach combined with sensory analysis was used to present the effects of different extraction methods (i.e., Pure Brew, V60, AeroPress, and French Press) on specialty graded Coffea arabica from Kenya. Partial Least Square Discriminant analysis and hierarchical clustering were applied as multivariate statistical tools in data analysis. The results showed good discrimination and a clear clustering of the groups of samples based on their volatile profiles. Similarities were found related to the filter material and shape used for the extraction. Samples extracted with paper filters (V60 and AeroPress) resulted in higher percentages of caramel-, and flowery-related compounds, while from metal filter samples (Pure Brew and French Press), more fruity and roasted coffees were obtained. Discriminant analysis allowed the identification of eight compounds with a high VIP (variable important in projection) discriminant value (i.e., >1), with 2-furanmethanol being the main feature in discrimination. Sensorial analyses were carried out through an expert panel test. The main evaluations revealed the French Press system as the lowest-scored sample in all the evaluated parameters, except for acidity, where its score was similar to V60. In conclusion, the data obtained from GC-MS analyses were in line with the sensorial results, confirming that the extraction process plays a fundamental role in the flavor profile of filter coffee beverages.

Rosehips, Rosa canina L. (Rosaceae family), have been used for a long time for their beneficial effects on health, and they are largely exploited in the food and nutraceutical supplement sectors. The aim of this work was to apply and optimize for the first time the microwave hydrodiffusion and gravity (MHG) extraction of rosehips, as a novel application of solvent-free microwave extraction, previously conducted in a similar way only on mulberry, strawberry, and onion. The optimization was performed through a central composite design (CCD) by evaluating the effect of the experimental parameters on the yield; total polyphenol, flavonoid, and anthocyanin contents; radical scavenging activity; and content of vitamin C in the obtained extracts. As a result, the water moistening pretreatment was clearly revealed to possess a pivotal role in the quality of the rosehip extracts. Among the evaluated responses, the yield, the anthocyanin content, and the antioxidant activity were well described by the statistical model. Notably, the optimized MHG extract was compared with the ones obtained by conventional solvent extraction showing higher amounts of vitamin C, polyphenols, flavonoids, and anthocyanins, while the traditional extracts performed better in terms of yield. In conclusion, MHG represents a promising alternative to standard extraction methods for obtaining rosehip extracts rich in vitamin C and antioxidant compounds. In this respect, the results of our research support the employment of MHG on an industrial level for the production of rosehip-based food supplements enriched in vitamin C.

Plasma activated water (PAW) recently received much attention as an alternative food preservation method. However, its effects on food quality are still scarce. This study evaluates the effect of PAW processing time on bioactive compounds of rocket-salad leaves including: 18 phenolic compounds, vitamin C, riboflavin, nicotinic acid, and nicotinamide. Moreover, the impact of PAW on both antioxidant (DPPH) and peroxidase (POD) activities was also investigated. This was performed using HPLC-DAD, HPLC-MS/MS, and spectrophotometric analysis. All treatments induced non-significant increases in total phenolic contents. However, depending on processing time, significant increases or decreases of individual phenolic compounds were observed. PAW-10 and -20 increased the ascorbic acid content to 382.76 and 363.14 mg/100 g, respectively, compared to control (337.73 mg/100 g). Riboflavin and nicotinic acid contents were increased significantly in PAW-20 (0.53 and 1.26 mg/100), compared to control (0.32 and 0.61 mg/100 g, respectively). However, nicotinamide showed non-significant increase in all treatments. Antioxidant activity improved significantly only in PAW-20, while peroxidase activity was reduced up to 36% in the longest treatment. In conclusion, PAW treatment could be an effective technique for rocket decontamination since it positively influenced the quality of rocket, improving the retention of polyphenols and vitamins.

Green coffee ( Coffee arabica and Coffee robusta ) is one of the most commonly traded goods globally. Their beans are enriched with polyphenols and numerous health benefits are associated with their consumption. The main aim of this work was to develop a new and fast analytical HPLC-MS/MS method to simultaneously determine six flavonoid polyphenolic compounds (quercetin, rutin, isorhamnetin, quercetin-3-glucouronide, hyperoside, and quercitrin) in 22 green coffee samples from six different geographical origins (Ethiopia, Brazil, Guatemala, Nicaragua, India and Colombia). In addition, by adjusting pH, temperature, solvent type, and extraction duration, several extraction methods such as acidic and alkaline hydrolysis, and extraction without hydrolysis were evaluated. The optimal extraction procedure in terms of recovery percentages (78.67-94.09%)was acidic hydrolysis at pH 2, extraction temperature of 60 °C, extraction solvent of 70% ethanol, and extraction duration of 1.5 h. Hyperoside (878-75 μg/kg) was the most abundant compound followed by quercitrin (408-38 μg/kg), quercetin (300-36 μg/kg), rutin (238-21 μg/kg), and quercetin-3-glucouronide (225-7 μg/kg), while isorhamnetin (34-3 μg/kg) showed the lowest amount. Overall, green coffee beans are rich in flavonoid polyphenolic compounds and could be used as part of a healthy diet.

Sweet chestnuts ( Castanea sativa Mill.) are highly prized nuts, and the consumption of fresh chestnuts is usually preceded by roasting, boiling, and frying. The aim of this work was to simultaneously analyze 29 polyphenolic compounds for the first time in raw, boiled, roasted, and fried chestnut seeds and shells using HPLC-MS/MS. Principal component analysis depending on the HPLC-MS/MS results showed that roasting, boiling, and frying affected the contents of 25 detected phenolic compounds in a unique way, of which the most notable phenolics were gallic acid, ellagic acid, and (+)-catechin. Additionally, total polyphenolic content (TPC) was measured via the Folin-Ciocalteu method, and TPC in seeds and inner and outer shells was increased in all treatments except for microwave-roasted seeds. Furthermore, the higher TPC in the inner and outer shells when compared to seeds supported their higher antioxidant activity (AOA) determined via the DPPH experiment. AOA of seeds was increased in all treatments, while the AOA of shells was higher in roasting and lower in boiling and frying treatments. The assessment of these changes is necessary so that chestnut seed consumption and the recycling of their shells as a natural source of antioxidants can be maximized.

Leonurus cardiaca L. (Lamiaceae) is a perennial herb distributed in Asia and Southeastern Europe and has been used in traditional medicine since antiquity for its role against cardiac and gynecological disorders. The polar extracts obtained from L. cardiaca aerial parts contain several compounds among which alkaloids, iridoids, labdane diterpenes, and phenylethanoid glycosides play a major role in conferring protection against the aforementioned diseases. On the other hand, the antioxidant activities and the enzyme inhibitory properties of these extracts have not yet been deeply studied. On the above, in the present study, crude and purified extracts were prepared from the aerial parts of L. cardiaca and have been chemically characterized by spectrophotometric assays and HPLC-DAD-MS analyses. Notably, the content of twelve secondary metabolites, namely phenolic acids (chlorogenic, caffeic, caffeoylmalic and trans -ferulic acids), flavonoids (rutin and quercetin), phenylethanoid glycosides (verbascoside and lavandulifolioside), guanidine pseudoalkaloids (leonurine), iridoids (harpagide), diterpenes (forskolin), and triterpenes (ursolic acid), has been determined. Furthermore, the extracts were tested for their antioxidant capabilities (phosphomolybdenum, DPPH, ABTS, FRAP, CUPRAC, and ferrous chelating assays) and enzyme inhibitory properties against cholinesterase, tyrosinase, amylase, and glucosidase. The purified extracts contained higher phytochemical content than the crude ones, with caffeoylmalic acid and verbascoside as the most abundant compounds. A linear correlation between total phenolics, radical scavenging activity, and reducing power of extracts has been found. Notably, quercetin, caffeic acid, lavandulifolioside, verbascoside, chlorogenic acid, rutin, and ursolic acid influenced the main variations in the bioactivities found in L. cardiaca extracts. Our findings provide further insights into the chemico-biological traits of L. cardiaca and a scientific basis for the development of nutraceuticals and food supplements.

Sterols, especially cholesterol and phytosterols, are important components of food lipids. During food processing, such as heating, sterols, like unsaturated fatty acids, can be oxidized. Protein modification by secondary products of lipid peroxidation has recently been demonstrated in food through a process called lipation. Similarly, this study was performed to assess, for the first time, the possibility of reactions between food proteins and sterol oxidation products in conditions relevant for food processing. Therefore, reaction models consisting of oxysterol (cholesterol 5α,6α-epoxide) and reactive amino acids (arginine, lysine, and methionine) were incubated in various conditions of concentration (0-8 mM), time (0-120 min), and temperature (30-180 °C). The identification of lysine adducts through thin-layer chromatography (TLC), high-performance liquid chromatography (HPLC) with a diode array detector (DAD), and electrospray ionization (ESI) mass spectrometry (MS) evidenced a reaction with lysine. Moreover, the HPLC-ESI with tandem mass spectrometry (MS/MS) analyses allowed observation of the compound, whose mass to charge ratio m/z 710.5 and fragmentation patterns corresponded to the reaction product [M + H] + between cholesterol-5α,6α-epoxide and the ε-amino-group of N α -benzoylglycyl-l-lysine. Moreover, kinetic studies between N α -benzoylglycyl-l-lysine as a model for protein-bound lysine and cholesterol 5α,6α-epoxide were performed, showing that the formation of lysine adducts strongly increases with time, temperature, and oxysterol level. This preliminary study suggests that in conditions commonly reached during food processing, sterol oxidation products could react covalently with protein-bound lysine, causing protein modifications.

In a world where an eco-friendlier approach is becoming more and more necessary, it is essential to reduce waste production and to reuse residues of the company's supply chain. Coffee silverskin (CS) and spent coffee ground (SCG), two by-products of coffee production, are important sources of bioactive compounds and, for this, some authors have proposed their reuse in the nutraceutical, food, and cosmetic sector. However, their potential enzyme inhibitory properties have been poorly investigated. Hence, the objective of the current work was to study the enzymatic inhibitory activities against acetylcholinesterase, butyrylcholinesterase, α-amylase, α-glucosidase, and tyrosinase of different extracts of CS and SCG. Before these in vitro bioassays, the phytochemical composition of each extract was investigated via colorimetric assays and HPLC-MS/MS analysis. In addition, the antioxidant activities were evaluated by different chemical approaches. SCG extracts contained a higher content of bioactive compounds, notably the SCG EtOH:H 2 O extract was the richest in caffeine and possessed the highest antioxidant activities. The hydroalcoholic and methanolic extracts were shown to be the most active against all tested enzymes, while the water extracts displayed lower activity. Our results showed a weak correlation between bioactive compounds and enzyme inhibitory effects, proving inhibitory activities likely due to non-phenolic molecules such as alkaloids and terpenoids. Obtained findings could be a starting point to develop novel nutraceuticals from CS and SCG.

The purpose of this work was the optimization of the extraction from spent coffee grounds, specifically 100% Arabica coffee blends, using a desirability approach. Spent coffees were recovered after the preparation of the espresso coffee under the typical conditions used in coffee bars with a professional machine. Spent coffee was subjected to different extraction procedures in water: by changing the extraction temperature (60, 80, or 100 °C) and the solvent extraction volume (10, 20, 30 mL for 1 gram of coffee) and by maintaining constant the extraction time (30 minutes). The ranges of the process parameters, as well as the solvent to be used, were established by running preliminary experiments not reported here. The variables of interest for the experimental screening design were the content of caffeine, trigonelline, and nicotinic acid, quantitatively determined from regression lines of standard solutions of known concentrations by a validated HPLC-VWD method. Since solvent extraction volumes and temperatures were revealed to be the most significant process variables, for the optimization of the extraction process, an approach based on Response Surface Methodology (RSM) was considered. In particular, a Box-Wilson Central Composite Design, commonly named central composite design (CCD), was used to find the optimal conditions of the extraction process. Moreover, the desirability approach was then applied to maximize the extraction efficiency by searching the optimal values (or at least the best compromise solution) for all three response variables simultaneously. Successively, the best extract, obtained in a volume of 20 mL of water at an extraction temperature of 80 °C, was analyzed for total phenol content (TPC) through the Folin-Ciocalteu assay, and the antioxidant capacities (AC) through the trolox equivalent (TE) antioxidant capacity (DPPH), ferric-ion reducing antioxidant parameter (FRAP), and radical cation scavenging activity and reducing power (ABTS). The TPC and the AC for spent coffee were high and comparable to the results obtained in previous similar studies. Then, the extract was evaluated by inductively coupled plasma mass spectrometry (ICP-MS), revealing that potassium was the most abundant element, followed by phosphorus, magnesium, calcium, sodium, and sulfur, while very low content in heavy metals was observed. Preliminary in vitro assays in keratinocyte HaCaT cells were carried out to assess the safety, in terms of cytotoxicity of spent coffee, and results showed that cell viability depends on the extract concentration: cell viability is unmodified up to a concentration of 0.3 mg/mL, over which it becomes cytotoxic for the cells. Spent coffee extract at 0.03 and 0.3 mg/mL showed the ability to reduce intracellular reactive oxygen species formation induced by hydrogen peroxide in HaCaT cells, suggesting its antioxidant activity at intracellular levels.

Chemical and sensory peculiarities of monovarietal extra virgin olive oils (MEVOOs) from the cultivars (cvs.) Ascolana tenera (ASC), Coroncina (COR), Mignola (MIG), Piantone di Mogliano (MOG), and Raggia (RAG) from Marche region (Italy) are investigated. Their polar phenolic substances and α-tocopherol are analysed through high performance liquid chromatography with different detectors. Volatile substances, fatty acid composition, and squalene are analysed by gas chromatography coupled to mass spectrometry (MS) and to the flame ionization detector, respectively. Total antioxidant activity and sensory analysis were also performed. MOG showed high squalene content (on average 0.88 ± 0.16 g/100 g), high relative amount of α-copaene among volatiles, and the highest oleic acid percentage. MIG had high α-tocopherol content (on average 350.0 ± 57.6 mg kg -1 ) and high α-farnesene in the volatile fraction. ASC showed the highest sensory quality and the lignan pinoresinol with higher concentration as compared to the other MEVOOs ( p < 0.05), which resulted in a possible chemical marker for this cv. RAG was characterized by the sensory note of almond, which corresponds to its highest ( E )-2-hexenal percentage. Sensory analysis and an antioxidant activity assay performed on a set of industrial extra virgin olive oils purchased in supermarkets, highlighted MEVOOs' superiority from these points of view. Principal component analysis displays the main characteristics of the cvs. investigated.

This study was undertaken to evaluate the nutraceutical potential of the Mela Rosa dei Monti Sibillini (MR), an ancient apple variety of the Sibillini Mountains, central Italy. The chemical profile of the apple's polyphenolic-rich extract (MRE) obtained from first- and second-choice samples using the Amberlite ® XAD7HP resin was analyzed by High Performance Liquid Chromatography with Diode-Array and Mass spectrometry (HPLC-DAD-MS) and 21 phytochemicals were quali-quantitatively determined. For comparative purposes, the polyphenol-rich extract of Annurca (ANE), a southern Italian variety, was analyzed. The antioxidant capacity of MREs was evaluated by Folin-Ciocalteu, 1, 1-diphenyl-2-picrylhydrazyl (DPPH), and 2, 2'-azino-bis (3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) assays. The inhibitory capacity of MREs for the enzymes α-glucosidase, lipase, monoamine oxidase A, tyrosinase, and acetylcholinesterase was also determined. The MREs showed higher polyphenolic and triterpene profiles than the ANE. Their radical scavenging activity was higher than that of ANE and comparable to the reference trolox. The MRE from the second-choice apples displayed higher contents of the 21 phytochemicals investigated. Either MRE from second-choice or first-choice samples showed enzymatic inhibition with IC 50 values higher than those of reference inhibitors but worthy of nutraceutical consideration. Taken together, these results show the potential of MRE as a source of bioactive compounds to be used for pharmaceutical, nutraceutical, and cosmeceutical applications has been confirmed.