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Keywords = LC-ESI/QTrap/MS/MS

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21 pages, 1047 KB  
Article
Development and Characterization of a Sunflower-Seed Press-Cake-Based Fermented Food Prototype
by Sofia Mendo, Beatrice Zignego, Francesca Bonazza, Fabio Masotti, Sara Casati, Sofia Vanerio, Roberto Foschino, Alessio Battistini and Ivano De Noni
Fermentation 2026, 12(4), 204; https://doi.org/10.3390/fermentation12040204 - 18 Apr 2026
Viewed by 1398
Abstract
Growing environmental and food security concerns have increased interest in circular strategies to valorize agri-food by-products. Sunflower-seed press cake (SSPC), a protein-rich residue from oil extraction, is largely underutilized despite its high nutritional and functional value. This study aimed to develop a fermented [...] Read more.
Growing environmental and food security concerns have increased interest in circular strategies to valorize agri-food by-products. Sunflower-seed press cake (SSPC), a protein-rich residue from oil extraction, is largely underutilized despite its high nutritional and functional value. This study aimed to develop a fermented plant-based food prototype (PBFP) from SSPC using Lactococcus lactis B12 and Penicillium camemberti, evaluating microbiological safety, chemical characteristics, and sensory acceptability. A blend containing 40% SSPC and 60% water was autoclaved, inoculated, and ripened for 4 weeks under controlled temperatures. Microbial counts, pH evolution, free amino acids, biogenic amines, volatile organic compounds (VOCs), cyclopiazonic acid (CPA) content, and sensory attributes were evaluated using cultural techniques, HPLC, HS-SPME/GC-MS, LC–ESI–MS/MS (QTRAP 4000), and sensory evaluation. L. lactis efficiently acidified the matrix (pH ≈ 4.5–4.9), ensuring microbial food safety, with high LAB counts (~109 CFU/g) and absence of pathogens (Listeria monocytogenes and Salmonella spp.) and hygienic markers < 2 log CFU/g (B. cereus, E. coli, and Enterobacteriaceae). Free amino acids decreased during fermentation, and no histamine or tyramine was detected. VOC analysis revealed diacetyl, acetoin, 2,3-butanediol, and 1-octen-3-ol, contributing to mild dairy-like notes. CPA was detected at 0.48 ng/g, well below levels reported in cheeses. Sensory evaluation showed no significant differences in overall intensity between inoculated and control blends, although qualitative descriptors indicated subtle changes in aroma and texture. These results demonstrate the feasibility of safely producing a fermented plant-based prototype from SSPC. Future studies should explore longer ripening times, additional microbial consortia, and strategies to enhance texture and aroma complexity. Full article
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14 pages, 3895 KB  
Article
In-Depth LC-ESI/HRMS-Guided Phytochemical Analysis and Antioxidant Activity Analysis of Eco-Sustainable Extracts of Cynara cardunculus (Carciofo di Paestum PGI) Leaves
by Antonietta Cerulli, Roberta Cuozzo, Maria Paola Melis, Gabriele Serreli, Monica Deiana, Milena Masullo and Sonia Piacente
Plants 2024, 13(24), 3591; https://doi.org/10.3390/plants13243591 - 23 Dec 2024
Cited by 10 | Viewed by 2053
Abstract
The Italian Carciofo di Paestum (C. scolymus) PGI, an artichoke variety from the Campania region, was investigated for its potential to reuse by-products for food supplements. EtOH:H2O 50:50 and 75:25 extracts of its leaves were analyzed for phenolic and [...] Read more.
The Italian Carciofo di Paestum (C. scolymus) PGI, an artichoke variety from the Campania region, was investigated for its potential to reuse by-products for food supplements. EtOH:H2O 50:50 and 75:25 extracts of its leaves were analyzed for phenolic and flavonoid content and antioxidant activity (TEAC: 1.90 and 1.81 mM of Trolox; DPPH IC50: 106.31 µg/mL and 128.21 µg/mL; FRAP: 1.68 and 1.58 mM FeSO₄/g extract). To further investigate the antioxidant potential, the ability of the two extracts to scavenge reactive species was assessed in Caco-2 cell cultures, showing a dose-dependent antioxidant capacity. To highlight metabolites responsible for the activity, LC-ESI/HRMSMS analysis was achieved, revealing 28 compounds (sesquiterpenes, megastigmanes, quinic acid and hydroxycinnamic acid derivatives, flavonoids, lignans, triterpenoid saponins, and polar fatty acids), of which structures were determined using 1D- and 2D-NMR analysis. In addition, quantitative determination of caffeoyl, dicaffeoyl, and quinic acid derivatives (CQAs) was performed through LC-ESI/QTrap/MS/MS, highlighting that the most abundant compound was 5-caffeoylquinic acid (6), with values of 9.310 and 7.603 mg/g extract in EtOH:H2O (75:25) and EtOH:H2O (50:50), respectively. The analysis showed that extracts were rich in bioactive compounds, suggesting their potential for development into antioxidant-based food supplements that may protect cells from oxidative stress and support overall wellness. Full article
(This article belongs to the Special Issue Bio-Active Compounds in Horticultural Plants)
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19 pages, 2252 KB  
Article
Spinacia oleracea L. Baby Leaves as a Source of Bioactive Principles: The Chemical Profiling of Eco-Sustainable Extracts by Using LC-ESI/HRMS- and 1H NMR-Based Metabolomics
by Antonietta Cerulli, Luciana Maria Polcaro, Milena Masullo and Sonia Piacente
Foods 2024, 13(22), 3699; https://doi.org/10.3390/foods13223699 - 20 Nov 2024
Cited by 7 | Viewed by 3510
Abstract
Spinacia oleracea L. cultivar platypus leaves are identified as a functional food due to their nutrient composition which promotes health beyond basic nutrition. Considering the increasing use of food supplements, S. oleracea baby leaves have been extracted by maceration, solid–liquid dynamic extraction (SLDE)-Naviglio, [...] Read more.
Spinacia oleracea L. cultivar platypus leaves are identified as a functional food due to their nutrient composition which promotes health beyond basic nutrition. Considering the increasing use of food supplements, S. oleracea baby leaves have been extracted by maceration, solid–liquid dynamic extraction (SLDE)-Naviglio, and ultrasound-assisted extraction (UAE) using EtOH and EtOH:H2O mixtures. The analysis of the extracts by using LC-ESI/HRMSMS revealed 42 compounds (flavonoids, polar lipid derivatives, and 20-hydroxyecdysone), along with primary metabolites, detected by NMR analysis. A principal component analysis (PCA) of LC-ESI/HRMS and NMR data was performed, revealing how 20-hydroxyecdysone and flavonoids, the specialized metabolites mainly responsible for the biological activity of S. oleracea leaves, occurred in the highest amount in the EtOH and EtOH:H2O (70:30, v/v) extracts obtained by SLDE-Naviglio extraction. 20-hydroxyecdysone was also quantified in all the extracts via LC-ESI/QTrap/MS/MS using the Multiple Reaction Monitoring (MRM) method. The EtOH extracts obtained by SLDE-Naviglio and maceration showed the highest content (82.16 and 81.27 mg/g extract, respectively). The total phenolic content (118.35–206.60 mg GAE/g), the flavonoid content (10.90–41.05 mg rutin/g), and the Trolox Equivalent Antioxidant Capacity (TEAC) (1.63–2.05 mM) of the extracts were determined. The EtOH:H2O (70:30, v/v) extract analyzed by using SLDE-Naviglio showed the highest phenolic and flavonoid content and radical scavenging activity. Full article
(This article belongs to the Special Issue Health Benefits of Antioxidants in Natural Foods)
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15 pages, 3839 KB  
Article
Chemical Profile and Antioxidant and Tyrosinase Inhibitory Activity of Chamaemelum nobile L. Green Extracts
by Luciana Maria Polcaro, Antonietta Cerulli, Francesco Montella, Elena Ciaglia, Milena Masullo and Sonia Piacente
Cosmetics 2024, 11(3), 94; https://doi.org/10.3390/cosmetics11030094 - 6 Jun 2024
Cited by 14 | Viewed by 5914
Abstract
The request for skin-whitening agents and bioactive principles able to control hyperpigmentation disorders is continuously growing. Chamomile (Matricaria chamomilla) is used as a remedy for skin diseases, but little is known about the ability of Roman chamomile (Chamaemelum nobile) [...] Read more.
The request for skin-whitening agents and bioactive principles able to control hyperpigmentation disorders is continuously growing. Chamomile (Matricaria chamomilla) is used as a remedy for skin diseases, but little is known about the ability of Roman chamomile (Chamaemelum nobile) to act as a skin-whitening agent. With the aim to investigate antioxidant and lightening potential, fresh aerial parts of C. nobile were extracted by maceration, ultrasound-assisted extraction, and solid–liquid dynamic (SLDE-Naviglio) extraction using EtOH/H2O mixtures. Moreover, 32 metabolites (flavonoids, sesquiterpenoids, amides, and polar fatty acids) were identified by liquid chromatography/mass spectrometry. Principal component analysis revealed how the extract EtOH/H2O 50% (Naviglio and long maceration), along with the extract EtOH/H2O 60% (maceration) were richest in flavonoids. All extracts were tested by TEAC and DPPH assays, and to determine their in vitro antioxidant activity, the DHR 123 probe–intracellular ROS assay in HaCaT cells, for some extracts, was performed. Moreover, their ability to exert a whitening effect was tested by analyzing their tyrosinase inhibitory activity. The quantitative determination of apigenin, known as a natural tyrosinase inhibitor, was performed by LC-ESI/QTrap/MS/MS using the multiple reaction monitoring (MRM) method. These results are promising for selecting an extraction method to obtain a sustainable product rich in bioactives. Full article
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16 pages, 2635 KB  
Article
Metabolite Profiling for Typization of “Rucola della Piana del Sele” (PGI), Eruca sativa, through UHPLC-Q-Exactive-Orbitrap-MS/MS Analysis
by Maria Assunta Crescenzi, Antonietta Cerulli, Paola Montoro and Sonia Piacente
Foods 2023, 12(18), 3384; https://doi.org/10.3390/foods12183384 - 9 Sep 2023
Cited by 11 | Viewed by 2811
Abstract
In August 2020, the Eruca sativa cultivar “Rucola della Piana del Sele” obtained from the European Union the prestigious PGI (protected geographical indication) label, which certifies the uniqueness of its characteristics and increases its prestige both nationally and, above all, internationally. This plant [...] Read more.
In August 2020, the Eruca sativa cultivar “Rucola della Piana del Sele” obtained from the European Union the prestigious PGI (protected geographical indication) label, which certifies the uniqueness of its characteristics and increases its prestige both nationally and, above all, internationally. This plant is recognized as a product of excellence, with a unique flavor and unmistakable aroma. Therefore, since there are no methods to characterize the PGI product, a metabolomic approach was applied to characterize E. sativa grown in the Piana del Sele and different geographical areas. As E. sativa has very wide cultivation, this study sought to compare the metabolite profiles of rocket grown in Piana del Sele, Bergamo, and Brescia, as well as in Switzerland, making a comparison also with the metabolite profile of E. sativa grown spontaneously. To determine the best procedure to distinguish “Rucola della Piana del Sele” from the others, different extraction procedures were carried out using different solvents and fresh or freeze-dried plant matrices. The different extracts were analyzed by liquid chromatography coupled with high-resolution mass spectrometry experiments, using chemometric analyses to identify biomarker metabolites that characterize the PGI product. The LC-ESI-Q-Exactive-MS/MS profiles of methanol and hydroalcoholic extracts of different cultivars of E. sativa were found to be rich in bioactive compounds such as glucosinolates, glycosylated flavonoids, fatty acids, and lipids. The LCMS data were analyzed by principal component analysis (PCA); the score scatter plot shows significant separation among Eruca samples grown in different geographical areas. In detail, loading the scatter plot revealed Eruca grown in Piana del Sele to be richer than other cultivars in glycosylated quercetin 3,3′,4′-O-triglucoside (7), quercetin-3,4′-O-diglucoside-3′-O-(6-sinapoyl-glucoside) (10), and quercetin diglucoside (30). Finally, considering the biological interest in erucin, the myrosinase product of glucoerucin, the latter was quantified in the extracts by LC-ESI/QTrap/MS/MS using the multiple reaction monitoring (MRM) method; E. sativa from Piana del Sele showed the highest content of glucoerucin. Full article
(This article belongs to the Section Food Analytical Methods)
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14 pages, 2309 KB  
Article
A Comparative UHPLC-Q-Trap-MS/MS-Based Metabolomics Analysis to Distinguish Foeniculum vulgare Cultivars’ Antioxidant Extracts
by Maria Assunta Crescenzi, Gilda D’Urso, Sonia Piacente and Paola Montoro
Molecules 2023, 28(2), 900; https://doi.org/10.3390/molecules28020900 - 16 Jan 2023
Cited by 6 | Viewed by 3711
Abstract
Among the environmental factors, seasonality is the one which most affects the metabolome of a plant. Depending on the harvest season, the plant may have a variable content of certain metabolites and thus may have different biological properties. Foeniculum vulgare is an annual plant [...] Read more.
Among the environmental factors, seasonality is the one which most affects the metabolome of a plant. Depending on the harvest season, the plant may have a variable content of certain metabolites and thus may have different biological properties. Foeniculum vulgare is an annual plant whose cultivation creates large amounts of waste rich in bioactive compounds. The present investigation was performed with the aim of determining the amount of biologically active compounds in F. vulgare wastes obtained from varieties of different seasonality. Ten polyphenolic compounds were quantified in the little stems and leaves of Tiziano, Pegaso, and Preludio cultivars by ultra performance liquid chromatography (UPLC) hyphenated to QTRAP mass spectrometry by using the MRM (multiple reaction monitoring) method. The antioxidant activity of hydroalcoholic extracts was then evaluated using TEAC and DPPH spectrophotometric assays, followed by a multivariate statistical analysis to determine the correlation between metabolite expression and antioxidant activity. The Preludio variety, grown in summer, showed a higher content of bioactive compounds, which guarantees it a better antioxidant power; kaempferol 3-O-glucuronide, quercetin 3-O-glucuronide, and quercetin 3-O-glucoside are the polyphenolic compounds that could be mainly responsible for the antioxidant effect of fennel. The PLS chemometric model, which correlated quantitative data obtained by a sensitive and selective LC-ESI-QTrap-MS/MS analysis of antioxidant activity, resulted in a selective tool to detect the compounds responsible for the activity shown by the extracts in chemical tests. Full article
(This article belongs to the Special Issue Natural Polyphenols in Human Health)
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19 pages, 1298 KB  
Article
Sustainable Extraction Methods Affect Metabolomics and Oxidative Stability of Myrtle Seed Oils Obtained from Myrtle Liqueur By-Products: An Electron Paramagnetic Resonance and Mass Spectrometry Approach
by Angela Fadda, Paola Montoro, Gilda D’Urso, Nicoletta Ravasio, Federica Zaccheria and Daniele Sanna
Antioxidants 2023, 12(1), 154; https://doi.org/10.3390/antiox12010154 - 9 Jan 2023
Cited by 11 | Viewed by 3507
Abstract
Myrtle liqueur production generates high amounts of by-products that can be employed for the extraction of bioactive compounds. Bio-based, non-toxic and biodegradable solvents (ethyl acetate and 2-methyltetrahydrofuran), and a mechanical extraction were applied to myrtle seeds, by-products of the liqueur production, to extract [...] Read more.
Myrtle liqueur production generates high amounts of by-products that can be employed for the extraction of bioactive compounds. Bio-based, non-toxic and biodegradable solvents (ethyl acetate and 2-methyltetrahydrofuran), and a mechanical extraction were applied to myrtle seeds, by-products of the liqueur production, to extract oils rich in phenolic compounds. The oils obtained were characterized for yield, peroxide value (PV), lipid composition, and total phenolic concentration (TPC). The phenolic profile of the oils, determined by LC-MS, the antioxidant activity, and the oxidative stability were also analyzed. A validated UHPLC-ESI-QTRAP-MS/MS analytical method in multiple reaction monitoring (MRM) mode was applied to quantify myricetin and its main derivatives in myrtle oils. The results pointed out clear differences among extraction methods on myricetin concentration. The oxidative stability of myrtle oils was studied with electron paramagnetic resonance (EPR) spectroscopy highlighting the effect of the extraction method on the oxidation status of the oils and the role of phenolic compounds in the evolution of radical species over time. A principal component analysis applied to LC-MS data highlighted strong differences among phenolic profiles of the oils and highlighted the role of myricetin in the oxidative stability of myrtle oils. Myrtle oil, obtained from the by-products of myrtle liqueur processing industry, extracted with sustainable and green methods might have potential application in food or cosmetic industries. Full article
(This article belongs to the Special Issue Antioxidants in Food and Cosmetics)
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9 pages, 780 KB  
Article
Sicilian Populations of Capparis spinosa L. and Capparis orientalis Duhamel as Source of the Bioactive Flavonol Quercetin
by Francesco Sgadari, Antonietta Cerulli, Rosario Schicchi, Natale Badalamenti, Maurizio Bruno and Sonia Piacente
Plants 2023, 12(1), 197; https://doi.org/10.3390/plants12010197 - 3 Jan 2023
Cited by 4 | Viewed by 3114
Abstract
The genus Capparis is a taxon of difficult delimitation that has several species and ecotypes due to its wide heterogeneity, its extreme phenotypic diversity, and the presence of intermediate forms linked to hybridization phenomena. The Sicilian territory hosts numerous wild and cultivated populations [...] Read more.
The genus Capparis is a taxon of difficult delimitation that has several species and ecotypes due to its wide heterogeneity, its extreme phenotypic diversity, and the presence of intermediate forms linked to hybridization phenomena. The Sicilian territory hosts numerous wild and cultivated populations of two spp. Capparis spinosa L. and Capparis orientalis Duhamel, which are ecologically and morphologically distinct. The caper has considerable interest and economic value for its medicinal properties, culinary uses, and cultivation characteristics. It is one of the foods with the highest quercetin content. Quercetin is a flavonol with antioxidant, anti-inflammatory, and immunostimulant properties. Recently, patents and clinical studies have highlighted the inhibitory effect of this compound against several SARS-CoV-2 enzymes (MPro, PLPro, and RdRp). Therefore, the aim of this study was to quantify the amount of quercetin in C. spinosa and C. orientalis by LC-ESI/QTrap/MS/MS and to correlate it with the pedoclimatic features. The results obtained showed that quercetin is more abundant in C. orientalis than in C. spinosa. The highest values of quercetin were recorded in C. orientalis flowers, leaves, and flower buttons of volcanic islands with southwest and east warm exposures. In conclusion, the data acquired can provide a good basis for further scientific investigations to support the identification of possible ecotypes as a source of quercetin for food or pharmaceutical purposes. Full article
(This article belongs to the Special Issue Natural Compounds in Plants and Their Anti-inflammatory Activity II)
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16 pages, 2345 KB  
Article
Metabolite Profiling of “Green” Extracts of Cynara cardunculus subsp. scolymus, Cultivar “Carciofo di Paestum” PGI by 1H NMR and HRMS-Based Metabolomics
by Antonietta Cerulli, Milena Masullo, Cosimo Pizza and Sonia Piacente
Molecules 2022, 27(10), 3328; https://doi.org/10.3390/molecules27103328 - 22 May 2022
Cited by 24 | Viewed by 4045
Abstract
Globe artichoke (Cynara cardunculus L. var. scolymus L.), is a perennial plant widely cultivated in the Mediterranean area, known for its edible part named capitula or heads. Its functional properties are related to its high levels of polyphenolic compounds and inulin. “Carciofo [...] Read more.
Globe artichoke (Cynara cardunculus L. var. scolymus L.), is a perennial plant widely cultivated in the Mediterranean area, known for its edible part named capitula or heads. Its functional properties are related to its high levels of polyphenolic compounds and inulin. “Carciofo di Paestum”, an Italian traditional cultivar, is a labeled PGI (Protected Geographical Indication) product of the Campania region, representing an important economic resource. So far, a few chemical investigations were performed on this cultivar, mainly focused on the analysis of methanol extracts. Due to the increasing use of food supplements, in this study, a comprehensive analysis of green extracts of “Carciofo di Paestum” PGI heads was performed. EtOH, EtOH: H2O (80:20, 70:30, 60:40) extracts, as well as infusions and decoctions prepared according to Pharmacopeia XII were analyzed by LC-ESI/QExactive/MS/MS. A total of 17 compounds corresponding to caffeoylquinic acid derivatives, phenolics, flavonoids, and terpenoids were identified. The extracts were further submitted to NMR analysis to highlight the occurrence of primary metabolites. Both LCMS and NMR data were analyzed by Principal Component Analysis (PCA), showing significant differences among the extraction methods. Moreover, 5-caffeoylquinic acid and 1,5-dicaffeoylquinic acid were quantified in the extracts by LC-ESI/QTrap/MS/MS using the Multiple Reaction Monitoring (MRM) method. Furthermore, the phenolic content, antioxidant activity, and α-glucosidase inhibitory activity of C. cardunculus var. scolymus “Carciofo di Paestum” extracts were evaluated. Full article
(This article belongs to the Special Issue Feature Papers in Food Chemistry)
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12 pages, 4409 KB  
Article
Identification of Metabolites of the Cardioprotective Alkaloid Dehydrocorydaline in Rat Plasma and Bile by Liquid Chromatography Coupled with Triple Quadrupole Linear Ion Trap Mass Spectrometry
by Huanyu Guan, Kaitong Li, Xiaoming Wang, Xiaomei Luo, Meifeng Su, Wenting Tan, Xiaoyan Chang and Yue Shi
Molecules 2017, 22(10), 1686; https://doi.org/10.3390/molecules22101686 - 10 Oct 2017
Cited by 15 | Viewed by 6225
Abstract
Dehydrocorydaline (DHC), a quaternary alkaloid from Corydalis yanhusuo, has been demonstrated to be the active constituent in the treatment of coronary heart disease. In this study, a high-performance liquid chromatography–electrospray ionization–triple quadrupole linear ion trap mass spectrometry (HPLC–ESI–QTRAP MS) technique was used [...] Read more.
Dehydrocorydaline (DHC), a quaternary alkaloid from Corydalis yanhusuo, has been demonstrated to be the active constituent in the treatment of coronary heart disease. In this study, a high-performance liquid chromatography–electrospray ionization–triple quadrupole linear ion trap mass spectrometry (HPLC–ESI–QTRAP MS) technique was used to identify DHC metabolites in plasma and bile after oral administration of DHC to rats. A total of 18 metabolites (M1 to M18) were identified and characterized by LC–MS/MS in the positive ion mode. These 18 metabolites were all present in rat bile, while only 9 were detected in plasma. O-demethylation, hydroxylation, di-hydroxylation, glucuronidation of O-demethyl DHC, sulfation of O-demethyl DHC and di-hydroxylation of dehydro-DHC were the major metabolic pathways of DHC. This is the first time that these metabolites of DHC have been identified in rat plasma and bile, which provides useful information for further analysis of the biotransformation of DHC and other quaternary protoberberine-type alkaloids. Full article
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