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Volutaria lippii (L.) Cass. ex Maire, syn. Centaurea lippii (L.), (Asteraceae) is a plant from the central region of Algeria, considerably distributed in all Mediterranean areas. Herein, the antioxidant activity of the three derived fractions [chloroform (CHCl3), ethyl acetate (EtOAc) and n-butanol (n-BuOH)] of the 70% methanol extract of the aerial parts (leaves and flowers), was assessed by using CUPRAC, ABTS, DPPH free radical scavenging, and β-carotene bleaching methods. The results obtained allowed to guide the fractionation of EtOAc and n-BuOH fractions by CC followed by purification by TLC and reverse phase HPLC. A guaianolide glucoside, 3β-hydroxy-11β,13-dihydrodehydrocostuslactone 8α-O-(6'-acetyl-β-glucopyranoside) (1), never reported in the literature, was isolated together with other known compounds (2–14). Their structures were elucidated by the extensive use of 1 D- and 2 D-NMR experiments along with ESI-MS analyses and with comparison with literature data.

Since the ethylacetate (EtOAc) extract of the roots of Zhumeria majdae had the potent cytotoxic effect (IC50 < 50 μg/ml) on three cancer cell lines; MCF-7, PC3 and MDAMB- 231, therefore the purpose of this study was the isolation of the responsible cytotoxic compounds from the plant. Isolation of the extract led to the identification of four diterpenoids named as lanugon Q (1), 12,16-dideoxy aegyptinone B (2), 12-deoxysalvipisone (3) and manool (4). The chemical structures have been determined on the basis of 1D and 2D NMR experiments. Compound 1 is reported for the first time in the plants of the Zhumeria genus. The results of cytotoxic and apoptotic evaluation revealed that compound 2 had a strong cytotoxic effect with the IC50 value of 15.90 μg/ml against MCF-7 cell lines. The sub-G1 peak in flow cytometry histogram of cells treated with the EtOAc extract and compound 2 showed the induction of apoptosis. Changes in the Bax/Bcl-2 ratio and cleavage of PARP were observed. It is to be noted that owing to the strong cytotoxic effect, the Z. majdae extract could be represented as a therapeutic agent against cancer.

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.

The new flavone glycosides tanoside I and II in addition to three known flavonoids and daucosterol were isolated from the Georgian endemic species Astragalus tanae Sosn. Their structures were elucidated as chrysoeriol-7-O-β-D-glucopyranosyl-4′ -O-α-L-rhamnopyranoside, chrysoeriol-4′ -O-α-Lrhamnopyranoside, kaempferol-3-O-β-D-glucopyranosyl(2→1)-O-α-L-rhamnopyranoside (kaempferol-3-O-β-D-neohesperidoside), tamarixin, apigenin, and β-sitosterol-3-O-β-D-glucopyranoside (daucosterol).

Melanoma is a highly malignant solid tumor characterized by an elevated growth and propagation rate. Since, often, melanoma treatment cannot prevent recurrences and the appearance of metastasis, new anti-melanoma agents need to be discovered. Salvia miltiorrhiza roots are a source of diterpenoid derivatives, natural compounds with several biological activities, including antiproliferative and anticancer effects. Seven diterpenoid derivatives were purified from S. miltiorrhiza roots and identified by NMR and MS analysis. Tanshinone IIA and cryptotanshinone were detected as the main components of S. miltiorrhiza root ethanol extract. Although their antitumor activity is already known, they have been confirmed to induce a reduction in A375 and MeWo melanoma cell growth. Likewise, salviolone has been shown to impair the viability of melanoma cells without affecting the growth of normal melanocytes. The underlying anticancer activity of salviolone has been investigated and compared to that of cryptotanshinone in A375 cells, showing an increased P21 protein expression in a P53-dependent manner. In that way, salviolone, even more than cryptotanshinone, displays a multitarget effect on cell-cycle-related proteins. Besides, it modulates the phosphorylation level of the signal transducer and activator of transcription (STAT)3. Unexpectedly, salviolone and cryptotanshinone induce sustained activation of the extracellular signal-regulated kinases (ERK)1/2 and the protein kinase B (Akt). However, the blockage of ERK1/2 or Akt activities suggests that kinase activation does not hinder their ability to inhibit A375 cell growth. Finally, salviolone and cryptotanshinone inhibit to a comparable extent some crucial malignancy features of A375 melanoma cells, such as colony formation in soft agar and metalloproteinase-2 activity. In conclusion, it has been shown for the first time that salviolone, harboring a different molecular structure than tanshinone IIA and cryptotanshinone, exhibits a pleiotropic effect against melanoma by hampering cell cycle progression, STAT3 signaling, and malignant phenotype of A375 melanoma cells.

Melanoma is a highly malignant solid tumor characterized by an elevated growth and propagation rate. Since, often, melanoma treatment cannot prevent recurrences and the appearance of metastasis, new anti-melanoma agents need to be discovered.

Helichrysum italicum is a medicinal plant from the Mediterranean area, widely used in traditional medicine for its anti-inflammatory, antibacterial and antioxidant properties and for its preventive effects on microcirculation diseases. Due to these properties, it finds large applications in cosmetic, food and pharmaceutical fields. Additionally, hydroalcoholic extracts and mother tinctures based on H. italicum represent products with a high commercial value, widely distributed not only in drug stores but also on on-line markets. The different extraction procedures used can greatly affect the fingerprints of the extracts, resulting in a different qualitative or quantitative profile of the chemical constituents responsible for biological activity. The aim of the present study was to characterize the composition of bioactive compounds present in water-ethanol and glycerol extracts of H. italicum derived food supplements. Metabolite profiles of the extracts were obtained by 1H NMR experiments and data were processed by multivariate statistical analysis to highlight differences in the extracts and to evidence the extracts with the highest concentrations of bioactive metabolites. In detail, this work highlights how derived food supplements of H. italicum obtained using ethanol-water mixtures ranging from 45% to 20% of ethanol represent the products with the highest amount of both primary (amino acids) and secondary metabolites including 3,4-dicaffeoylquinic acid (9), chlorogenic acid (10), 3,5-dicaffeoylquinic acid (11), and kaempferol 3-O-glucopyranoside (12). Moreover, it is evident that the use of an ethanol-water mixture 20:80 is the most suitable method to afford the highest number of phenolic compounds, while food-derived supplements obtained by glycerol extraction are characterized by a high amount of β-glucose and α-glucose and a low content of phenolic compounds.

The flavone C-glycosides namely apigenin-7-O-β- d -glucopyranosyl-8-C-β- d -glucopyranoside (1) and apigenin-8-C-α- l -rhamnopyranosyl-(1→2)-O-β- d -glucopyranoside (2), along with p-methoxycinnamic acid (3), vaccaroside A (4), vaccaroside D (5), vaccaroside E (6) and abscisic acid glucose ester (7) were isolated from the methanol extract of the aerial parts of Vaccaria pyramidata. Structure elucidation of compounds 1-7 was accomplished by the extensive use of 1D- and 2D NMR experiments along with HR-ESI-MS. The structures of 1-2 have been confirmed by theoretical study of the 1H, 13C chemical shifts and UV data. In addition, Ionization Potential (IP) and Bond Dissociation Enthalpy (BDE) were used to evaluate the theoretical antioxidant activity of compounds 1 and 2. TD-DFT method (time-dependent density functional) was used to calculate the electronic absorption spectra of compounds 1 and 2 from optimized structures in methanol and the orbitals involved in the electronic transition were elucidated.

With the aim to explore the ability of diarylheptanoids to reduce oxidative changes in human plasma proteins, a phytochemical investigation of the MeOH extract of

The Italian “Marrone di Roccadaspide” (Castanea sativa), a labeled Protected Geographical Indication (PGI) product, represents an important economic resource for the Italian market. With the aim to give an interesting opportunity to use chestnuts by-products for the development of nutraceutical and/or cosmetic formulations, the investigation of burs and leaves along with chestnuts of C. sativa, cultivar “Marrone di Roccadaspide”, has been performed. The phenolic, tannin, and flavonoid content of the MeOH extracts of “Marrone di Roccadaspide” burs, leaves, and chestnuts as well as their antioxidant activity by spectrophotometric methods (1,1-diphenyl-2-picrylhydrazyl (DPPH), Trolox Equivalent Antioxidant Capacity (TEAC), and Ferric Reducing Antioxidant Power (FRAP) have been evaluated. Furthermore, a cell-based antioxidant in vitro test along with in vitro assays for the evaluation of the ability to reduce nuclear factor-kappa B (NF-κB) activation and nitric oxide (NO) production have been carried out. In order to identify the secondary metabolites responsible for the high phenolic content and the strong antioxidant activity shown by leaves and burs extracts, and to highlight the differences between their chemical composition, the analysis of the metabolite profile of the MeOH extracts obtained from both by-products and chestnuts by liquid chromatography coupled to electrospray ionization and multiple-stage linear ion-trap and Orbitrap high-resolution mass spectrometry (LC-(-)ESI/LTQOrbitrap/MS/MS) has been performed. LC-MS analysis allowed the identification of different classes of specialized metabolites including hydrolyzable tannins, flavonoids, ellagic acid and phenol glucoside derivatives, and triterpenoids as well as polar lipids. Our results show how the antioxidant activity of the extracts can be correlated to their high tannins and flavonoids content while polar lipids occurring in the MeOH extract of the leaves could contribute to determining its higher anti-inflammatory activity.

Pouteria lucuma Ruiz and Pav., known as the ‘Gold of the Incas’ or ‘lucuma’, is a subtropical fruit belonging to the Sapotaceae family, with a very sweet flavor, used to prepare cakes, ice creams as well as in the baking and dairy industries. To date, the content of primary metabolites is known, but little information is reported about the composition in specialized metabolites. Moreover, no study is reported on skin which represent an important agricultural waste due to the high demand for lucuma. In order to have a preliminary metabolite profile of Pouteria lucuma, the extracts of pulp and skin have been analyzed by LC-ESI/LTQOrbitrap/MS/MS in negative ion mode. The careful analysis of the accurate masses, of the molecular formulas and of the ESI/MS spectra allowed to identify specialized metabolites belonging to phenolic, flavonoid and polar lipid classes. The LC-MS/MS analysis guided the isolation of compounds occurring in the pulp extract whose structures have been characterized by spectroscopic methods including 1D- and 2D-NMR experiments and ESI-MS analysis. Furthermore, the phenolic content of the extracts along with the antioxidant activity of extracts and isolated compounds was evaluated.

From the MeOH extract of the aerial parts of Scutellaria brevibracteata subsp. subvelutina 12 secondary metabolites including eight iridoid glycosides (1-8), three flavonoids (9-11) and one phenylethanoid glycoside (12) were isolated. Their structures were elucidated as catalpol (1), globularin (2), scutellarioside II (3), picroside III (4), pensteminoside (5), 8-epiloganic acid (6), albidoside (7), agnucastoside B (8), hispidulin (9), luteolin 7-O-glucuronide (10), hispidulin 7-O-glucuronide (11) and martynoside (12) by using extensive NMR and HR-MS analysis. All compounds are being reported for the first time from S. brevibracteata subsp. subvelutina while compound 5 is new for Lamiaceae family. The chemotaxonomic importance of the isolates was discussed in the detail. All the isolates were evaluated for their in vitro anti-inflammatory activities via their inhibitory actions on the release of nitrite oxide and IL-6 from LPS-induced RAW 264.7 macrophage cells. Compounds 9 and 11 exhibited significant NO reducing capacity at 100 μM concentration comparable to the positive controls, indomethacin and L-NAME. Moreover, 2, 9 and 10 significantly suppressed the release of IL-6 at the same concentration better than the positive controls.

Perovskia artemisioides is a perennial and aromatic plant distributed in the Baluchestan region of Iran. In the present work, an n-hexane extract of P. artemisioides aerial parts showed excellent capabilities to both inhibit the formation of biofilms by different Gram-positive and Gram-negative pathogens and block the cell metabolism within microbial biofilms. To correlate the activity of the extract with the biologically active compounds present, first an analytical approach based on LC-HRMS/MSn was carried out. The metabolite profile obtained guided the isolation of 21 compounds, among which two sesquiterpenes (8 and 9) and one diterpene (10) were found to be new. The antimicrobial activity of the isolated compounds was evaluated by determining how they were able not only to reduce the growth of different Gram-positive and Gram-negative human bacteria and phyto-pathogens but also to inhibit the formation of biofilms by these bacteria and affect the metabolism of microbial cells present within the biofilms. With the aim of correlating the activity exhibited by the extract with the concentration levels of the constituent compounds, a quantitative determination was carried out by an analytical approach based on LC-ESI/QTrap/MS.

With the aim to explore the ability of diarylheptanoids to reduce oxidative changes in human plasma proteins, a phytochemical investigation of the MeOH extract of Corylus avellana leaves was perfom...

Okra is a vegetable crop very popular in tropical, subtropical, and warm temperate regions of the world for its edible fruit. Nowadays, this species can be easily found in European local markets, as a basic ingredient in many local and traditional dishes. Considering the extensive and spread use of okra fruits, to achieve deep insight on its chemical composition the analysis of the polar extract by high-performance liquid chromatography coupled to multiple-stage linear ion-trap and orbitrap high-resolution mass spectrometry in negative electrospray ionization mode was carried out. By this approach, 39 metabolites belonging to different polar lipid classes, such as oxylipins, phospholipids, glycolipids, and sphingolipids, were putatively identified for the first time in A. esculentus. Moreover, LC-HRMS/MS analyses guided the isolation and characterization by NMR experiments of 19 specialized metabolites belonging to phenolic acid and flavonoid classes, 8 of them never reported before in A. esculentus. Finally, antioxidant activity and inhibition of α-glucosidase activity were assayed, suggesting a good anti-oxidant anti-hyperglycemic activity for okra fruit.

Preparations of comfrey (Symphytum officinale L.) roots are used topically to reduce inflammation. Comfrey anti-inflammatory and analgesic properties have been proven in clinical studies. However, the bioactive compounds associated with these therapeutic activities are yet to be identified. An LC&ndash, ESI&ndash, Orbitrap&ndash, MSn metabolite profile of a hydroalcoholic extract of comfrey root guided the identification of 20 compounds, including a new arylnaphthalene lignan bearing a rare &delta, lactone ring, named comfreyn A. Its structure was determined using extensive 2D NMR and ESI&ndash, MS experiments. Additionally, the occurrence of malaxinic acid, caffeic acid ethyl ester, along with the lignans ternifoliuslignan D, 3-carboxy-6,7-dihydroxy-1-(3&prime, 4&prime, dihydroxyphenyl) -naphthalene, globoidnan A and B, and rabdosiin was reported in S. officinale for the first time. These results helped to redefine the metabolite profile of this medicinal plant. Finally, caffeic acid ethyl ester and comfreyn A were found to significantly inhibit E-selectin expression in IL-1&beta, stimulated human umbilical vein endothelial cells (HUVEC), with EC values of 64 and 50 &micro, M, respectively.

The genus Scabiosa (Caprifoliaceae) is represented by 80 species, widely used as medicinal plants for their positive effects on human diseases. on the basis of the interesting biological activity shown by Scabiosa spp., the phytochemical investigation of Scabiosa sicula L., never investigated before, was carried out. An initial LC-MS profile of the MeOH extract of S. sicula whole plant guided the isolation of 34 compounds, of which the structures were unambiguously elucidated by NMR analysis as phenolic compounds and triterpene saponins, among which eight undescribed compounds. Moreover, the total phenolic content of S. sicula methanol extract has been evaluated. on the basis of the pharmacological activities reported for Scabiosa species the antioxidant activity of the methanol extract was tested by TEAC and DPPH assays. Finally, the alpha-glucosidase inhibitory activity of the methanol extract was assayed, showing an IC50, value (49 mu g/mL) comparable to that exerted by acarbose (90 mu g/mL), used as positive control., TUBITAK 2219 International PostDoctoral Research Fellowship ProgrammeTurkiye Bilimsel ve Teknolojik Arastirma Kurumu (TUBITAK) [1059B191700874], This work was supported by TUBITAK 2219 International PostDoctoral Research Fellowship Programme (Grant number: 1059B191700874).

The endoplasmic reticulum (ER) is a dynamic organelle essential for intracellular homeostasis maintenance, controlling synthesis, the folding of secreted and membrane-bound proteins, and transport of Ca2+. During cellular stress, ER dysfunction leads to the activation of unfolded protein response (UPR) due to accumulated misfolded proteins in the ER. This condition is referred as ER stress. Mitochondria and ER form a site of close contact (the mitochondria-associated membrane, MAM) which is a major platform exerting important physiological roles in the regulation of intracellular Ca2+ homeostasis, lipid metabolism, mitochondrial fission, autophagosome formation, and apoptosis progression. Natural products have been receiving increasing attention for their ability to interfere with ER stress. Research works have focused on the capacity of these bioactive compounds to induce apoptosis by activating ER stress through the ER stress-mediated mitochondrial apoptotic pathway. In this review we discuss the role of natural products in the signaling communication between ER and mitochondria, focusing on the effects induced by ER stress including Ca2+ permeability transition and UPR signaling (protein kinase R-like ER kinase/mitofusin 2).

Silene species are known for their use in traditional medicine in treating several diseases. To the authors' knowledge there is no report on the chemical composition of S. odontopetala. Therefore, the phytochemical investigation of the methanol extract of S. odontopetala was carried out, leading to the isolation of six undescribed oleanane-type glycosides along with the known saponin azukisaponin IV. Their structures were elucidated by the analysis of 1D and 2D-NMR experiments, along with mass spectrometry analysis. the cytotoxic activity of oleanane-type saponins was evaluated against a small panel of cancer cell lines, including PC-3 (prostate carcinoma cells), MCF-7 (breast cancer cells), A549 (alveolar basal carcinoma cells), and HeLa (cervical carcinoma cells). Furthermore, the activity of isolated compounds against a normal cell line HEK-293, used for assessing their cytotoxicity, was evaluated., TUBITAKTurkiye Bilimsel ve Teknolojik Arastirma Kurumu (TUBITAK) [114Z226]; Ege University Research FoundationEge University [2012 Fen 033]; project "Fighting Cancer resistance: Multidisciplinary integrated Platform for a technological Innovative Approach to Oncotherapies (Campania Oncotherapies)", This work was supported by the project "Fighting Cancer resistance: Multidisciplinary integrated Platform for a technological Innovative Approach to Oncotherapies (Campania Oncotherapies)". the authors are grateful to TUBITAK (114Z226), and to the Ege University Research Foundation (2012 Fen 033) for financial support.

Okra is a vegetable crop very popular in tropical, subtropical, and warm temperate regions of the world for its edible fruit. Nowadays, this species can be easily found in European local markets, as a basic ingredient in many local and traditional dishes. Considering the extensive and spread use of okra fruits, to achieve deep insight on its chemical composition the analysis of the polar extract by high-performance liquid chromatography coupled to multiple-stage linear ion-trap and orbitrap high-resolution mass spectrometry in negative electrospray ionization mode was carried out. By this approach, 39 metabolites belonging to different polar lipid classes, such as oxylipins, phospholipids, glycolipids, and sphingolipids, were putatively identified for the first time in A. esculentus. Moreover, LC-HRMS/MS analyses guided the isolation and characterization by NMR experiments of 19 specialized metabolites belonging to phenolic acid and flavonoid classes, 8 of them never reported before in A. esculentus. Finally, antioxidant activity and inhibition of α-glucosidase activity were assayed, suggesting a good anti-oxidant anti-hyperglycemic activity for okra fruit.

In Italy a particularly valuable chestnut is “Marrone di Roccadaspide”, a protected geographical indication (PGI) product, deriving from a Castanea sativa cultivar, typical of Salerno province in Campania region. As chestnut industrial processes yield a large amount of shell by-products, in this study the possibility to retrain this waste food as potential source of bioactives was investigated. The ability of “Marrone di Roccadaspide” shell MeOH extract to modulate the pro-inflammatory transcriptional factor NF-κB after LPS stimulation, along with the antioxidant activity by a cell-based in vitro test, were evaluated. To correlate the NF-κB inhibition (67.67% at 5 μg/mL) and the strong antioxidant activity to the chemical composition, an analytical approach based on LC-ESI/LTQOrbitrap/MS/MSn along with NMR characterization of isolated compounds was developed. The identification of hydrolysable and condensed tannins, along with flavonoids, phenol glucosides, ellagic acid derivatives, and triterpenoids was accomplished. The most representative compounds were quantitatively analyzed by LC-ESI/QTrap/MS/MS, showing bartogenic acid as the compound occurring in the highest amount (103.08 mg/100 g shells). With the aim to explore the possibility to employ chestnut shells as suitable source of bioactives for the preparation of functional ingredients, the chemical composition and the antioxidant activity of “eco-friendly” extracts (EtOH and EtOH:H2O 7:3) was finally evaluated, showing a high superimposability of the EtOH:H2O (7:3) extract to the MeOH extract.

Lettuce (Lactuca sativa L.) is a popular vegetable with the health-enhancing properties determined by high levels of antioxidant polyphenols as chlorogenic acids and other derivatives of caffeic acid or flavonoids. In this study, changes in the phenolic compound profiles in the lettuce leaves induced by application of CaCl2 before harvest and cold storage were studied. For the first time quantitative analysis of individual phenolic compounds on the basis of standards isolated from lettuce leaves was performed. Compounds were identified using HPLC, LC-MS, 1H and 13CNMR techniques. The dominant compounds were 2,3-dicaffeoyltartaric (2,3-diCTA), 5-O-caffeoylquinic (5-OCQA) and caffeoyltartaric (CTA) acids, with content of 5.7, 2.5 and 0.981 mg/g DM, respectively. The levels of individual phenolic compounds, total phenolics and antioxidant activity (DPPH assay) in plants treated by CaCl2 were determined throughout the storage period (7 and 14 days) at 4 °C. To ascertain the relationship between the content of individual compounds, total phenols, antioxidant activities and storage time, Pearson’s correlation analysis was used. The best correlation between the storage length and compound concentration was observed for 2,3-diCTA (R2 = 0.866) and caffeoylmalic acid (CMA) (R2 = 0.750). Application of CaCl2 (0.05M) on lettuce resulted in an increase in the levels of CTA, 2.3-diCTA and 5-OCQA about 120, 65 and 57%, respectively, compared to the control stored for 7 days in the same conditions and had a favourable effect on the antioxidant activity (R2 = 0.985). The present paper shows that CaCl2 may be used as an agent that influences the stability of health-promoting compounds of cold-stored lettuce.

Corylus avellana L. (Betulaceae) leaves, consumed as infusion, are used in traditional medicine, for the treatment of hemorrhoids, varicose veins, phlebitis, and edema due to their astringent, vasoprotective, and antiedema properties. In previous works we reported from the leaves of Corylus avellana cv. "Tonda di Giffoni" diarylheptanoid derivatives, a class of plant secondary metabolites with a wide variety of bioactivities. With the aim to give an interesting and economically feasible opportunity to C. avellana leaves as source of functional ingredients for pharmaceutical and cosmetic formulations, "green" extracts were prepared by employing "eco-friendly" extraction protocols as maceration, infusion and SLDE-Naviglio extraction. Metabolite profiles of the extracts were obtained by 1H NMR experiments and data were processed by multivariate statistical analysis to highlight differences in the extracts and to evidence the extracts with the highest concentrations of bioactive metabolites. Based on the NMR data, a total of 31 compounds were identified. The metabolite variation among the extracts was evaluated using Principle Component Analysis (PCA) and Partial Least Squares-Discriminant Analysis (PLS-DA). Furthermore, the total phenolic content of the extracts was measured by Folin-Ciocalteu colorimetric assay and the antioxidant activity of extracts was assayed by the spectrophotometric tests DPPH• and ABTS and by an in vitro test based on the evaluation of cellular reactive oxygen species production stimulated by pyocyanin.

Prunus dulcis leaves have been reported to exert some biological activity, in particular potent free radical-scavenging capacity, but so far there is limited information on their chemical composition. With the aim to achieve deep insight on the chemical constituents of the leaves of P. dulcis cultivars "Toritto" and "Avola", the most appreciated in Italy, an approach based on liquid chromatography-mass spectrometry (LC-MS) combined with isolation and structure elucidation of pure compounds by Nuclear Magnetic Resonance (NMR) analysis was carried out. Results allowed to detect in cv. Toritto leaves phenolics, terpenoids and a cyanogenic glycoside. Successively, various solvent systems were chosen to afford different extracts and an approach based on principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) from LC-MS data sets highlighted eco-friendly methods as selective in extracting phenolics and glycosides. Comparison of LC-MS profiles of the MeOH extracts of cv. Toritto and cvs. Avola (Pizzuta, Fascionello and Romana) leaves and evaluation of their phenolic contents and antioxidant activity were also carried out.

Rationale Actinocephalus divaricatus (Eriocaulaceae) is an important source of income for rural communities as it is sold as an ornamental plant. To date, no investigation has been conducted concerning the chemical composition and biological studies of the aerial parts of A. divaricatus. Methods The methanolic extract of the aerial parts of this species was chemically characterized. We applied an analytical dereplication approach based on Liquid Chromatography coupled to High-Resolution Orbitrap Mass Spectrometry in order to develop, identify and define rapidly the metabolite fingerprint of the aerial parts of A. divaricatus. Biological in vitro antitumor tests were undertaken using breast and lung cell lines of mice and humans. Results High-Resolution Mass Spectrometry (HRMS) allowed the fast determination of 30 compounds, which comprised three different classes of compounds: naphthopyranones, flavonoids and saponins. Chromatographic fractionation of the crude methanolic extract validated these results, since it led to the isolation of compounds belonging to the aforementioned classes of compounds, including new acyl glycosylated flavonoids (6-hydroxy-7-methoxyquercetin-3-O-(2"-O-acetyl)-β-D-glucopyranoside and 6-hydroxy-7-methoxyquercetin-3-O-(6"-O-acetyl)-β-D-glucopyranoside), which were fully characterized by Nuclear Magnetic Resonance and Mass Spectrometry experiments, and a known triterpenic saponin (3-O-β-D-glucuronopyranosyl-30-norolean-12,20(29)-dien-28-O-β-D-glucopyranosyl ester). Biological assays indicated that the methanolic extract of the capitula exhibited the best in vitro cytotoxicity against MCF7 cells (human breast cancer). Conclusions The HRMS technique enabled us to identify several classes of compounds. In addition, saponins were identified for the first time in plants belonging to the Eriocaulaceae family. Thus, the essential contribution of this work lies in the new elements it brings to the taxonomic discussion which the Actinocephalus genus as a distinct genus of the Paepalanthus. The results obtained show that the methanolic extract of the capitula could be a promising source of bioactive fractions and/or compounds that may contribute towards breast cancer treatment.

The genus Scabiosa (Caprifoliaceae) is represented by 80 species, widely used as medicinal plants for their positive effects on human diseases. On the basis of the interesting biological activity shown by Scabiosa spp., the phytochemical investigation of Scabiosa sicula L., never investigated before, was carried out. An initial LC-MS profile of the MeOH extract of S. sicula whole plant guided the isolation of 34 compounds, of which the structures were unambiguously elucidated by NMR analysis as phenolic compounds and triterpene saponins, among which eight undescribed compounds. Moreover, the total phenolic content of S. sicula methanol extract has been evaluated. On the basis of the pharmacological activities reported for Scabiosa species the antioxidant activity of the methanol extract was tested by TEAC and DPPH assays. Finally, the α-glucosidase inhibitory activity of the methanol extract was assayed, showing an IC

Garcinol, a polyisoprenylated benzophenone isolated from Garcinia genus, has been reported to inhibit eukaryotic topoisomerase I and topoisomerase II at concentrations comparable to that of etoposi...