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The circular economy is gaining attention around the world as a sustainable approach to tackling environmental problems, promoting more responsible management of resources. The aim of this work is the valorization of grape pomace as a waste product of agrifood chain. We prepared decoction (DC), ultrasound-assisted and microwave-assisted extracts (UAE and MAE respectively) of grape pomace, determining their phytochemical profile (using HPLC-ESI-Q-TOF-MS), antioxidant activity and enzyme inhibitory effects. Then, the results were compared with those of raisins and several edible berries already present in the market. Grape pomace extracts presented the highest total phenolic content (62-68 mg gallic acid equivalents/g; mg GAE/g), whereas the concentrations in the other berries were 4-43 mg GAE/g. These results were in agreement with the higher antioxidant activity and tyrosinase inhibition observed in grape pomace compared with the other berries, except for the metal chelating activity. The main compounds in grape pomace extracts were flavonoids (particularly quercetin glycosides), followed by organic acids (citric, isocitric and gallic acids). These results open new perspectives in the development of food supplements and nutraceuticals based on grape pomace extracts., Competing Interests: Declaration of competing interest The authors declare no competing financial interests., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

The Cucurbita genus has been widely used in traditional medicinal systems across different countries. In this study, we aimed to investigate the chemical composition, antioxidant properties, enzyme inhibitory, and cytotoxic effects of methanol and aqueous extracts obtained from the aerial parts, seeds, and fruit shells of Cucurbita okeechobeensis. Antioxidant properties were assessed using various chemical methods, including radical quenching (DPPH and ABTS), reducing power (CUPRAC and FRAP), metal chelation, and phosphomolybdenum assays. The extracts' enzyme inhibitory effects were tested against cholinesterase, amylase, glucosidase, and tyrosinase, whereas different cancer cell lines were used for the cytotoxicity study. The chemical composition, evaluated by HPLC-ESI-MS n , showed that the most abundant compounds were flavonoids (mainly quercetin glycosides) followed by phenolic acids (mostly caffeic acid derivatives). The aerial parts displayed stronger antioxidant ability than the seed and fruit shells, in agreement with the highest content in phytochemicals. In addition, the methanol extracts presented the highest bioactivity and content in phytochemicals; among them, the extract of the aerial part exhibited significant cytotoxic effects on cancer cell lines and induced apoptosis. Overall, our results suggest that C. okeechobeensis is a valuable source of bioactive compounds for the pharmaceutical and nutraceutical industries., (© 2024 Deutsche Pharmazeutische Gesellschaft.)

Extraction and mineral processing, as well as the waste generated by old abandoned mining sites, are the main sources of contamination of water bodies and lands by potentially toxic elements (PTEs). The common carp (Cyprinus carpio Linnaeus 1758) has been reported to be a good ecological indicator of environmental pollution in water bodies. Hence, we evaluated the concentration of eleven PTEs (As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, and Zn) in different tissues of common carp in two reservoirs of the province of Jaén, southern Spain: El Tranco de Beas (S1) and La Fernandina (S2). We also assessed the concentration of PTEs in water and sediment samples. We used inductively coupled plasma mass spectrometry for all the collected samples. We found high concentrations of As and Fe in water in the S2 reservoir, above the maximum limits allowed by the sanitary criteria in Spain; however, the analysis of sediments indicated low ecological risk in S1 and moderate ecological risk for As in S2. The concentration of PTEs in common carp was higher in the S2 reservoir, exceeding the permissible limits in the case of As, Cd, Pb, and Zn. As and Cd showed higher concentrations in the kidney; Cu, Fe, and Zn showed higher concentrations in the liver; and Pb and Mn presented higher concentrations in the gill and gill bone. There was a good correlation between the concentrations found in water/sediment samples and those in common carp, corroborating its usefulness as a good ecological indicator, allowing the detection of environmental pollution and inferring previous or current anthropogenic activities such as mining., (© 2023. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

We propose a modification of terbium-sensitized luminescence (TSL) by means of the introduction of nanoparticles to improve the sensitivity and selectivity of the analytical methods. TSL detection is usually based on the complexation between fluorescent organic compounds (the analytes) and terbium. The organic compound is then excited, and, after an energy transfer towards terbium, the latter emits the luminescence signal. Here, the modification consists of the introduction of nanoparticles (carbon quantum dots, CQDs) into the system. The carboxylic groups of CQDs react with terbium, providing an interesting time-resolved luminescence probe. We applied this system for the determination of the neonicotinoid imidacloprid (IMID). When IMID was introduced in the terbium-CQDs system, the luminescent signal ( λ exc / λ em of 256/545 nm) was quenched, proportionally to IMID concentration in the range of 100-2500 ng·mL -1 , obtaining a limit of detection of 30 ng·mL -1 . A method detection limit of 0.9 mg·kg -1 was reached in caneberries, thus complying with the maximum residue level of 5 mg·kg -1 established by Codex Alimentarius. We performed recovery experiments in caneberries (blackberries, blueberries, raspberries, and mulberries), obtaining recovery yields close to 100% in all cases. These results show that the use of terbium ions-nanoparticles luminescence probes can be useful for screening purposes in quality control laboratories., Competing Interests: The authors declare that they have no conflicts of interest., (Copyright © 2023 Eulogio J. Llorent-Martínez et al.)

Bioactive phytoconstituents have been increasingly investigated for their potential human health benefits. Corema album (L.) D. Don, an Ericaceae, reportedly has antioxidant, antimicrobial and anticancer properties. Aiming at enhancing its nutraceutical potential, we performed a spectrochemical analysis of hydroethanolic extracts from C. album leaves. We report on changes in the antioxidant activity of the extracts, as well as in the accumulation of key phytoconstituents (namely phenolic compounds), in female and male samples, throughout three harvesting seasons (February, July, and October). For each extract, the antioxidant activity was assessed by different spectrophotometric methods. Simultaneously, attenuated total reflectance Fourier transform mid-infrared spectroscopy (FTIR-ATR), and high-performance liquid chromatography - electrospray ionisation - quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q-TOF-MS), were used to identify and monitor variations in the composition of phenolic compounds in the extracts. The main compounds identified were epicatechin, laricitrin-O-hexoside isomers, and myricetin-O-hexoside isomers. Significant differences were found in the composition and relative abundance of the compounds of interest, according to sex and season. Overall, a trend was observed whereby phenolic content and antioxidant activities were higher in males and increased between the earlier and the latest harvests. Based on these results, we may conclude that late summer or early autumn harvests are preferable when aiming at the highest yearly content of bioactive compounds. Additionally, it should be considered that extracts from male individuals typically display higher antioxidant activities. Ultimately, our understanding of C. album in the context of nutraceutical applications is benefited from the quantitative and qualitative portrait provided here, thus promoting its relevance as a source of bioactive compounds., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Author(s). Published by Elsevier B.V. All rights reserved.)

Secamone afzelii (Roem. & Schult.) K. Schum (family Asclepiadaceae) is a creeping woody climber used to treat ailments in many traditional medicine systems. The present study aims to examine the antioxidant and enzyme inhibition activities of S. afzelii leaf using different compositions of methanol-water mixture as an extraction solvent. The extracts were characterized by HPLC-ESI-MS n in terms of chemical compounds. The in silico results show that compound 23 (quercitrin) has the higher docking scores among the selected substances and the MD simulation revealed that the interactions with the enzymatic pocket are stable over the simulation time and strongly involve the tyrosinase catalytic Cu atoms. All together the results showed that both 80% and 100% methanolic extracts contained significantly ( p < 0.05) the highest total phenolics content while the highest content of total flavonoids was significantly ( p < 0.05) extracted by 100% methanol. About 26 compounds were tentatively identified by HPLC-ESI-MS n and 6 of them were quantified using standards. Results showed that the extracts were rich in flavonoids with a relatively high abundance of two kaempferol glycosides comprising 60% of quantified compounds. The 100% and 80% methanol extracts recorded significantly ( p < 0.05) the highest total antioxidant, DPPH and ABTS activity as well as tyrosinase and ⍺-amylase inhibitory activities. The best significant ( p < 0.05) cholinesterase inhibitory activity and reducing capacity of Fe +++ and Cu ++ was recorded from the 80% methanolic extract while 100% ethanolic extract gave the highest significant ( p < 0.05) butyrylcholinesterase inhibitory activity. The best glucosidase activity was observed in the 50% and 80% methanolic extracts. Although the water extract displayed the least total phenolics and flavonoids content and consequently the lowest antioxidant and enzyme inhibition activity, it displayed significantly ( p < 0.05) the highest chelating power. In conclusion, these results demonstrated the richness of S. afzelii leaf as a potential source of bioactive compounds for the food industry, for the preparation of food supplements and functional foods.

Polygonum hydropiperoides Michx. is an Asian native plant species that is also widely distributed in the Americas. Despite its traditional uses, P. hydropiperoides is scarcely scientifically exploited. This study aimed to chemically characterize and investigate the antioxidant and antibacterial activities of hexane (HE-Ph), ethyl acetate (EAE-Ph), and ethanolic (EE-Ph) extracts from aerial parts of P. hydropiperoides . The chemical characterization was performed through HPLC-DAD-ESI/MS n . The antioxidant activity was assessed by the phosphomolybdenum reducing power, nitric oxide inhibition, and the β-carotene bleaching assays. The antibacterial activity was determined by the minimal inhibitory concentration (MIC) and the minimal bactericidal concentration followed by the classification of the antibacterial effect. Chemical characterization revealed the expressive presence of phenolic acids and flavonoids in EAE-Ph. An increased antioxidant capacity was revealed in EAE-Ph. Regarding antibacterial activity, EAE-Ph showed weak to moderate property against 13 strains tested with MIC values ranging from 625 to 5000 µg/mL, with bactericidal or bacteriostatic effects. Glucogallin and gallic acid stand out as the most relevant bioactive compounds. These results suggest that P. hydropiperoides is a natural source of active substances, supporting this species' traditional use.

Ravenala madagascariensis is a widely known ornamental and medicinal plant, but with a dearth of scientific investigations regarding its phytochemical and pharmacological properties. Hence, these properties were appraised in this study. The DPPH (154.08 ± 2.43 mgTE/g), FRAP (249.40 ± 3.01 mgTE/g), CUPRAC (384.57 ± 1.99 mgTE/g), metal chelating (29.68 ± 0.74 mgEDTAE/g) and phosphomolybdenum assay (2.38 ± 0.07 mmolTE/g) results demonstrated that the aqueous extract had the most prominent antioxidant activity, while the methanolic extract displayed the best antioxidant potential in the ABTS assay (438.46 ± 1.69 mgTE/g). The HPLC-ESI-Q-TOF-MS-MS analysis allowed the characterization of 41 metabolites. The methanolic extract was the most active against acetylcholinesterase. All extracts were active against the alpha-amylase and alpha-glucosidase enzymes, with the ethyl acetate extract being the most active against the alpha-amylase enzyme, while the methanolic extract showed the best alpha-glucosidase inhibition. A plethora of metabolites bonded more energetically with the assayed enzymes active sites based on the results of the in silico studies. R. madagascariensis extracts used in this study exhibited cytotoxicity against HT29 cells. The IC 50 of the methanolic extract was lower (506.99 ug/mL). Based on the heat map, whereby flavonoids were found to be in greater proportion in the extracts, it can be concluded that the flavonoid portion of the extracts contributed to the most activity.

This study documents for the first time the phytochemical composition and biological activities of Tambourissa peltata Baker, an endemic plant from Mauritius. Phytochemical extraction was performed using ethyl acetate, methanol and distilled water as solvents. The phytochemical composition was determined through HPLC-MS and other standard assays. The DPPH, ABTS, FRAP, CUPRAC and phosphomolybdenum assays were employed for the determination of the antioxidant potential, whereas cell viability assays were used to determine the cytotoxicity. The highest phenolic and phenolic acid contents were obtained in the aqueous extract (179.91 ± 0.67 gallic acid equivalents/g and 55.74 ± 1.43 caffeic acid equivalents/g). The highest quantity of flavonoids was obtained in the ethyl acetate extract (28.97 ± 0.46 rutin equivalents/g). The methanolic extract was the highest source of flavonols (33.71 ± 0.13 mg catechin equivalents/g). A total of 34 phytochemicals were identified, mainly proanthocyanidins and flavonoid glycosides. The highest antioxidant activity in DPPH (973.40 ± 5.65 mg TE (Trolox equivalents)/g), ABTS (2030.37 ± 40.83 mg TE/g), FRAP (1461.39 ± 5.95 mg TE/g), CUPRAC (1940.99 ± 20.95 mg TE/g) and phosphomolybdenum (8.37 ± 0.23 mmol TE/g) assays was recorded for the aqueous extract. The ethyl acetate extract was the most active metal chelator. The highest acetylcholinesterase inhibitor was the methanolic extract, whereas the ethyl acetate extract was the most active against BChE. The tyrosinase enzyme was most inhibited by the methanolic extract. Alpha-amylase and glucosidase were most inhibited by the aqueous extract. The methanolic extract was capable of inducing cell cytotoxicity to the human colorectal carcinoma without damaging normal cells. T. peltata warrants further attention from the scientific community given its multifaceted biological properties.

Moringa oleifera has been reported to possess a high number of bioactive compounds; hence, several food supplements are commercially available based on it. This work aimed to analyze the phytochemical composition and antioxidant activity of commercial food supplements. The phenolic composition of methanolic extracts was determined by using high-performance liquid chromatography with diode-array and electrospray ionization mass spectrometric detection (HPLC-DAD-ESI-MS n ), and the antioxidant activity was assessed by ABTS ·+ and DPPH assays. Thirty-three compounds were identified, and all the main compounds were quantified, observing that the main contribution to the phenolic profile was due to kaempferol and quercetin glucosides. The antioxidant activity in both assays agreed with the phenolic content: the higher the phenolic levels, the higher the antioxidant activity. The obtained results were compared with those previously published regarding Moringa oleifera leaves to establish the potential benefits of food supplement consumption in the diet.

In this study, the methanolic and infusion extracts of two species, Thymbra capitata and Thymus sipyleus subsp. rosulans , were tested for their chemical composition and biological abilities (antioxidant, enzyme inhibitory and anti-inflammatory effects). The extracts yielded total phenolic and flavonoid contents in the range of 83.43-127.52 mg GAE/g and 9.41-46.34 mg RE/g, respectively. HPLC analysis revealed rosmarinic acid to be a major component of the studied extracts (15.85-26.43%). The best ABTS radical scavenging ability was observed in the methanol extract of T. capitata with 379.11 mg TE/g, followed by in the methanol extract of T. sipylus (360.93 mg TE/g). In the CUPRAC assay, the highest reducing ability was also found in the methanol extract of T. capitata with 802.22 mg TE/g. The phosphomolybdenum ability ranged from 2.39 to 3.61 mmol TE/g. In terms of tyrosinase inhibitory effects, the tested methanol extracts (83.18-89.66 mg KAE/g) were higher than the tested water extracts (18.74-19.11 mg KAE/g). Regarding the BChE inhibitory effects, the methanol extracts were active on the enzyme while the water extracts showed no inhibitory effect on it. Overall, the methanolic extracts showed better enzyme inhibition compared to the infusion extracts. Molecular docking also showed the selected exhibited potential binding affinities with all enzymes, with a preference for cholinesterases. Additionally, the extracts were effective in attenuating the LPS-induced increase in COX-2 and IL-6 gene expression in isolated colon, thus indicating promising anti-inflammatory effects. The preliminary results of this study suggest that these species are good natural sources of antioxidants and also provide some scope as enzyme inhibitors, most likely due to their bioactive contents such as phenolic acids, and thus can be exploited for different applications related to health promotion and disease prevention.

Ricinodendron heudelotii stem bark is commonly used in Cameroonian traditional medicine to treat cardiovascular diseases such as hypertension. The present study was designed to investigate the antihypertensive and antioxidant properties of the aqueous extract of Ricinodendron heudelotii in salt-induced hypertensive rats. Analysis by HPLC-ESI-Q-TOF-MS was used to identify various chemical components of the extract. A total of thirty rats were used for each test. High-salt hypertension was induced in rats by oral administration of NaCl for 12 weeks. Mean blood pressure (MBP) and heart rate (HR) were monitored by noninvasive methods. Oral administration of Ricinodendron heudelotii significantly ( p < 0.01) reduced the increase of mean blood pressure (23.12%, 26.14%, and 24.34%) and heart rate (31.19%, 31.09%, and 26.98%), respectively, at the doses of 40, 20, and 6 mg/kg, compared to the hypertensive group. All the doses tested significantly reduced or/and ameliorated biochemical and oxidative stress parameters. Histological analysis showed that Ricinodendron heudelotii restored renal disorders induced by the administration of salt. The aqueous extract of Ricinodendron heudelotii exerts a cardioprotective effect, and the antihypertensive activity seems associated with an improvement in antioxidant status. Overall, the results justify and support the traditional use of Ricinodendron heudelotii., Competing Interests: The authors declare that they have no conflicts of interest., (Copyright © 2022 Jacquy Joyce Wanche Kojom et al.)

Artemisia verlotiorum Lamotte is recognized medicinally given its long-standing ethnopharmacological uses in different parts of the world. Nonetheless, the pharmacological properties of the leaves of the plant have been poorly studied by the scientific community. Hence, this study aimed to decipher the phytochemicals; quantify through HPLC-ESI-MS analysis the plant’s biosynthesis; and evaluate the antioxidant, anti-tyrosinase, amylase, glucosidase, cholinesterase, and cytotoxicity potential on normal (NIH 3T3) and human liver and human colon cancer (HepG2 and HT 29) cell lines of this plant species. The aqueous extract contained the highest content of phenolics and phenolic acid, methanol extracted the most flavonoid, and the most flavonol was extracted by ethyl acetate. The one-way ANOVA results demonstrated that all results obtained were statistically significant at p < 0.05. A total of 25 phytoconstituents were identified from the different extracts, with phenolic acids and flavonoids being the main metabolites. The highest antioxidant potential was recorded for the aqueous extract. The best anti-tyrosinase extract was the methanolic extract. The ethyl acetate extract of A. verlotiorum had the highest flavonol content and hence was most active against the cholinesterase enzymes. The ethyl acetate extract was the best α-glucosidase and α-amylase inhibitor. The samples of Artemisia verlotiorum Lamotte in both aqueous and methanolic extracts were found to be non-toxic after 48 h against NIH 3T3 cells. In HepG2 cells, the methanolic extract was nontoxic up to 125 µg/mL, and an IC50 value of 722.39 µg/mL was recorded. The IC50 value exhibited in methanolic extraction of A. verlotiorum was 792.91 µg/mL in HT29 cells. Methanolic extraction is capable of inducing cell cytotoxicity in human hepatocellular carcinoma without damaging normal cells. Hence, A. verlotiorum can be recommended for further evaluation of its phytochemical and medicinal properties.

The aim of this study was to characterise the phenolic profile and evaluate the antioxidant activity of aqueous and methanol leaf extracts from Euonymus japonicus Thunb., a species of flowering plant in the Celastraceae family. Liquid chromatography (HPLC) with diode array and electrospray-tandem mass spectrometry (DAD-ESI-MS n ) detection was used to characterise and quantify phenolic compounds. Thirty-two compounds were detected; among them, flavonoids (mainly quercetin and kaempferol glycosides) were the most abundant compounds in both extracts. The results obtained for DPPH and ABTS assays in the extracts were in agreement with the highest content of phenolics in the methanol extract.

The use of plants and their metabolites stands as a promising option to tackle parasitic infections by gastrointestinal nematodes (GIN) in integrated control strategies. Still, the influence of environmental and phenological factors, and their interactions, in the wild on the metabolomics and biological properties of target plant species, is often disregarded. In this work, we hypothesized that variations in the anthelmintic (AH) properties and chemical composition of extracts from the salt tolerant species Cladium mariscus L. Pohl (sawgrass) may be influenced by seasonal factors and organ-parts. To test this hypothesis, acetone/water extracts were prepared from dried biomass obtained from aerial organs collected from sawgrass in consecutive seasons and tested against Haemonchus contortus and Trichostrongylus colubriformis by the larval exsheathment inhibition assay (LEIA) and egg hatching inhibition assay (EHIA). To ascertain the role of plant organ, the activity of leaves and inflorescences extracts from summer samples was compared. The role of polyphenols in the anthelmintic activity depending on GINs and fluctuations across seasons and plant organs was assessed using polyvinylpolypyrrolidone (PVPP), coupled with an in-depth chemical profiling analysis using high-performance liquid chromatography completed with electrospray ionization mass spectrometric detection (HPLC-ESI-MSn). Main differences in anthelmintic activities were observed for summer and autumn samples, for both assays. Moreover, inflorescences' extracts were significantly more active than those from leaves against both parasite species on EHIA and against H. contortus on LEIA. Application of PVPP totally inhibit the AH effects based on EHIA and only partly for LEIA. Non-treated PVPP extracts were predominantly composed of flavan-3-ols, proanthocyanidins, luteolin and glycosylated flavonoids, while two flavonoid glycosides were quantified in all PVPP-treated samples. Thus, the activity of such compounds should be further explored, although some unknown metabolites remain to be identified. This study reinforces the hypothesis of the AH potential of sawgrass and of its polyphenolic metabolites uses as nutraceutical and/or phytotherapeutic drugs., Competing Interests: The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest., (Copyright © 2022 Oliveira, Lima, Llorent-Martínez, Hoste and Custódio.)

We propose a modification of lanthanide-sensitized luminescence (LSL) to increase the selectivity and sensitivity of analytical methods based on this detection. LSL consists in the formation of complexes of lanthanide ions and organic compounds. Then, an intramolecular energy transfer occurs from the excited state of the ligand (organic analyte) to the emitting level of the lanthanide. The utilization of luminescent nanoparticles (carbon quantum dots, CQDs) in LSL systems can enhance their sensitivity and selectivity. CQDs can react with lanthanide ions through their carboxylic groups. These systems can thus be used as time-resolved luminescent probes. Propineb (PPN), a well-known dithiocarbamate fungicide, has been selected as the target analyte to show the advantages of using CQDs in LSL systems. The method proposed is based on the quenching produced by PPN in europium-CQDs luminescence, obtaining a detection limit of 0.03 μg mL -1 PPN and a method detection limit of 3 mg kg -1 in capers (bud and fruit), fulfilling the maximum residue limit in these samples (25 mg kg -1 ). The results showed that the use of nanoparticles in LSL systems may provide novel and simple analytical methods for the screening of contaminants in the agri-food sector., (Copyright © 2022 The Authors. Published by Elsevier B.V. All rights reserved.)

Cathissa reverchonii (formerly Ornithogalum reverchonii ) is a threatened species, constituting an endemism present in the south of Spain and northern Morocco. In Spain, it is only found in two disjoint populations in the region of Andalusia. The determination of its chemical composition and the influence that environmental factors have on it can contribute significantly to the development of appropriate protection and conservation plans. However, there are no previous reports about this species to date. Consequently, this research aimed to study the phenolic composition and antioxidant activity of C. reverchonii and to assess the influence of environmental factors on the phenolic profile and bioactivity. The vegetal material was collected in seven places inhabited by the two separate populations in Spain. The phenolic composition of methanolic extracts of the species was determined by HPLC-ESI-Q-TOF-MS, and the antioxidant activity was assessed by DPPH and ABTS assays. Fifteen compounds were characterized in the extracts of the aerial parts of C. reverchonii , revealing differences in the phytochemical profile between both populations analyzed, mainly in the saponin fraction. The main phenolics were flavone di- C -glucoside (lucenin-2), followed by a quercetin-di- C -glucoside. The composition of the extracts of C. reverchonii and their radical scavenging power were compared with those of other species of the genus Ornithogalum L., revealing significant differences between the latter and the genus Cathissa .

Kitchen gardening is considered a way to reconnect with agriculture and complement the cereal-based relief food offered to refugees in East Africa. This work aimed at profiling mineral content of okra in four refugee camps and settlements located in Ethiopia and Uganda and its contribution to adequate intake (AIs) or recommended dietary allowances (RDAs) for young children and pregnant and lactating women (PLW). The study also evaluated the applicability of portable X-ray fluorescence (PXRF) as compared with inductively coupled plasma mass spectrometry (ICP-MS) for mineral profiling of okra powder samples. The contents of minerals (mg kg -1 ) from the ICP-MS readings were in the following ranges: K (14,385-33,294), Ca (2610-14,090), P (3178-13,248), Mg (3896-7986), Cu (3.81-19.3), Fe (75.7-1243), Zn (33-141) and Mn (23.1-261). Regardless of geographic origin, at low-end consumption probability (17 g day -1 for young children and 68 g day -1 for PLW), okra could contribute ˂ 15% (2.7-12.9%) AI for macro-minerals (K and Ca). In addition, the contributions to RDA values for Fe and Zn, elements of known public health interest, ranged from 4.5 to 34.7% for young children. Interestingly, regression lines revealed strong agreement between ICP-MS and PXRF readings for Mn and Zn, with R 2 values > 0.91. This information is useful in support of nutrition-sensitive kitchen gardening programs through scaling culturally important crops in refugee settings., Supplementary Information: The online version contains supplementary material available at 10.1007/s42452-021-04898-6., Competing Interests: Conflict of interestThe authors declare no conflict of interest., (© The Author(s) 2021.)

Strategies to reduce dependence on synthetic drugs for the treatment of gastrointestinal nematodes (GIN) infections in ruminants include the search for novel anthelmintic scaffolds on plants, yet salt-tolerant plants remain overlooked. This study aims to evaluate the in vitro anthelmintic properties of selected salt-tolerant plants against GIN, and identify the potential bioactive secondary metabolites involved. For that purpose, 80% acetone/water extracts were prepared from dried biomass of aerial organs of nine salt-tolerant plant species and tested against Haemonchus contortus and Trichostrongylus colubriformis by the Larval Exsheathment Inhibition Assay (LEIA) and Egg Hatching Inhibition Assay (EHIA). Pistacia lentiscus, Limoniatrum monopetalum, Cladium mariscus and Helychrisum italicum picardi were the most active in both GIN and life stages. To investigate the role of polyphenols in the anthelmintic activity, four selected extracts were treated with polyvinylpolypyrrolidone (PVPP), and non-treated and treated samples were further characterized by high-performance liquid chromatography with electrospray ionization mass spectrometric detection (HPLC-ESI-MS n ). While polyphenols seem responsible for the EHIA properties, they are partially accountable to LEIA results. Several phenolics involved in the anthelmintic effects were identified and discussed. In sum, these species are rich sources of anthelmintic compounds and, therefore, are of major interest for nutraceutical and/or phytotherapeutic applications against GIN in ruminants., (© 2021. The Author(s).)

Grape pomace is commonly considered a waste product of monovarietal red wine production. Methods: HPLC-DAD analysis was performed to determine the polyphenol and flavonoid contents of all the extracts obtained from Montepulciano d'Abruzzo red wine and grape skins whereas, GC-MS was applied to the determination of fatty acid composition in grape seeds oil. Biological characterization involves antioxidant and antimicrobial assays for all the extracts and seeds oil; Their ability to inhibit α-glucosidase, α-amylase, α-tyrosinase, and ChE enzymes was also detected, together with anti-inflammatory activity on wine, grape skin extracts, and seeds oil by lipoxygenase (5-LOX) and LPS-stimulated macrophage release assays. Data indicate significative polyphenols content (199.31 ± 7.21 mgGAE/g), antioxidant (CUPRAC assay (1036.98 mgTE/g)), enzymatic inhibition (α-tyrosinase: 151.30 ± 1.20 mgKAE/g) and anti-inflammatory activities for wine-organic extract 2, while the antimicrobial activity of grape skin decoction is higher than those reported by wine extracts on three bacterial strains. Interestingly only dealcoholized wine and wine-aqueous extract exerts inhibitory effects on α-glucosidase (20.62 ± 0.23 mmolACAE/g and 19.81 ± 0.03 mmolACAE/g, respectively), while seeds oil is rich in oleic and linoleic acids. These results confirm the strong antioxidant properties of Montepulciano d'Abruzzo grape pomace, suggesting the potential use of this waste product as functional food supplements in the human diet and in cosmeceutics.

The phenolic composition and mineral content of Cornezuelo, Cornicabra and Picual olive fruit varieties were investigated during olive ripening in two different harvesting seasons (2017/2018 and 2018/2019). Phytochemical profiles were evaluated by high-performance liquid chromatography (HPLC) with diode-array and mass spectrometry detection. Mineral contents were determined by inductively coupled plasma-mass spectrometry (ICP-MS). Twenty-five compounds were characterized and the main ones quantified. These compounds corresponded mostly to secoiridoids, the main ones being oleuropein, oleoside/secologanoside, oleoside-11-methylester, and oleuropein and comselogoside isomers. Total phenolic contents reached the highest values between December and January, coinciding with the usual harvesting date. This trend was observed in both harvesting seasons, although higher phenolic contents were recorded in season 2018/2019. This was due to the different weather conditions, which caused a lower olive production in season 2017/2018. No clear tendency was observed between mineral content and harvest time in any of the studied seasons. The highest concentration of total phenolics was obtained in Cornezuelo variety (840 mg/100 g) in January 2019 (season 2018/2019). Picual and Cornicabra varieties reached concentrations of 670 mg/100 g and 530 mg/100 g, respectively, also in the last harvesting dates of season 2018/2019.

In this work, we compared the phenolic composition and antioxidant capacity of methanolic extracts of raw and steamed aerial parts of Portulaca oleracea L. Two new cyclo-dopa amides were identified, named oleraceins X and Y, along with six known ones (oleraceins A, B, C, N, J, and U). Compounds identification and quantification were done by high-performance liquid chromatography with diode array and mass spectrometry detections. The most abundant compounds were phenolic alkaloids (oleraceins), and the main quantified compounds were isocitric and citric acids, with concentrations of 500-550 and 440-600 mg/100 g dried extract, respectively. The study of both the influence of the steaming process in Portulaca oleracea L. and total phenolic content and radical scavenging assays (ABTS ·+ and DPPH) were also carried out. The total individual phenolic content of raw Portulaca decreased from 1380 mg/100 g DE to 1140 mg/100 g DE after the steaming process. The antioxidant capacity in ABTS and DPPH assays decreased approximately 50 and 40%, respectively, after samples were cooked by steaming. The raw extracts presented the highest concentration of bioactive compounds, as well as higher antioxidant and radical scavenging values.

The traditional Ethiopian flat bread, injera, is a regular component of daily diets in Ethiopia and Eritrea. This bread is also popular among urban refugees particularly Eritreans in Addis Ababa. The levels of metal(loid)s in 40 composite (120 sub-samples) injera samples, representing 4 types of market establishments in Addis Ababa, were determined using inductively coupled plasma-mass spectrometry (ICP-MS) and portable X-ray fluorescence (PXRF). For ICP-MS analysis, the accuracy of the method was evaluated by the analysis of a certified reference material and recovery experiments. It was found that the correlations between the mean levels of Al and Fe and between Al and Mn in injera were highly significant (p < 0.001). It was also found that 1.5 fresh injeras would cover 48-75% of recommended dietary allowance (RDA) for Mg, 17-21% of RDA for K, 19-23% of RDA for Ca, and 60-72% of RDA for P for an adult group aged between 19 and 50. Daily intakes of Al, Fe, and Mn were found to be above the provisional tolerable daily intake (PTDI)/maximum tolerable daily intake (MTDI) values. The mean target hazard quotient (THQ) values for Fe and Mn were greater than 1. The total THQ values varied from 6.52 to 8.53 among market establishments. Estimating carcinogenic risk due to exposure to As, Cr, and Pb indicated that perennial injera consumers might remain at cancer risk. This would further escalate if other staple food items and spices are considered. Hence, there is a need for home-based strategies to reduce extrinsic soil-Al-Fe-Mn in injera/tef batter.

Accurate-controlled sized graphene quantum dots (GQDs) have been used as an analytical nanoprobe for detecting curcumin as a function of the photoluminescent quenching upon increasing concentrations of the analyte. Regarding the importance of curcumin nanoparticles in nutraceutical food, the analytical method described herein was also proven for the discrimination of curcumin remaining in free solution from that encapsulated into water-soluble nanomicelles of ca. 11 nm. This recognition is based on the displacement of GQD emission when interacting with both curcumin species. Maximum emission wavelength of GQDs suffers a gradual quenching as well as a red-shifting upon increasing concentrations of free curcumin (from 458 to 490 nm, exciting at 356 nm). On the other hand, in the presence of nanocurcumin, GQD photoluminescent response only displays a quenching effect (458/356 nm). The sensitivity of the described method in terms of detection limits was 0.3 and 0.1 μg mL -1 for curcumin and nanocurcumin, respectively. The applicability of the photoluminescent probe for the quantification and discrimination between both curcumin environments was demonstrated in nutraceutical formulations namely functional food capsules and fortified beverages such as ginger tea. Graphical abstract.

In this work, we report the phenolic composition and bioactivity of the aerial parts of three species of Sarcocapnos ( S. enneaphylla , S. pulcherrima , and S. saetabensis ) to study their potential as sources of bioactive compounds to revalorize them and contribute to the conservation of these plant species. Samples were collected in different locations in the province of Jaén (southeast of Spain), and qualitative and quantitative analyses of phenolic compounds were performed by high-performance liquid chromatography with diode array and mass spectrometry detection. S. enneaphylla presented the highest concentration of phenolic compounds (58 mg/g DE). The most abundant compound in S. enneaphylla and S. saetabensis was rutin (35 mg/g DE and 11.7 mg/g DE, respectively), whereas isorhamnetin-O-rutinoside was dominant in S. pulcherrima (11.5 mg/g DE). Several assays were performed to evaluate the potential bioactivity of the three species of Sarcocapnos . These assays included antioxidant and radical scavenging (ABTS and DPPH), reducing power (CUPRAC and FRAP), phosphomolybdenum and metal chelating, and enzyme inhibitory activity (acetylcholinesterase, amylase, butyrylcholinesterase, glucosidase, and tyrosinase). In general, all methanolic extracts presented the highest phenolic and flavonoid contents, as well as the highest radical scavenging, antioxidant, and enzyme inhibitory properties. This relationship between phenolics and bioactivity was confirmed by multivariate analysis., Competing Interests: The authors declare that they have no conflicts to interest., (Copyright © 2020 María del Pilar Fernández-Poyatos et al.)

Rice is one of the most important foods in the world due to its high nutritional value and production. Quinclorac, a selective herbicide, is one of the most detected pesticide residues in rice crops according to pesticide monitoring studies. Common methods for the determination of quinclorac in rice are very time-consuming and labour-intensive, so it is important to develop alternative sensitive and simple analytical methods able to detect quinclorac in food samples. Here we propose a fluorometric method for the screening of this herbicide at excitation/emission wavelengths of 238/358 nm/nm, respectively. A modified QuEChERS method was selected for sample treatment due to its simplicity and high recovery yields. The proposed method presents a detection limit of 2.5 ng mL -1 and satisfactory precision. Recovery experiments were performed in different kinds of rice (white and brown) at or below the Maximum Residue Limit established in European Union (5 mg kg -1 ), obtaining values close to 100%. All these characteristics ensure that the proposed method fulfils the requirements for its application in food control.

Anacamptis pyramidalis (L.) Rich. forms part of the Orchidaceae family that is highlyvalued for its horticultural as well as therapeutic benefits. The present study set out to investigatethe inhibitory activity of A. pyramidalis tubers against key biological targets for the management oftype 2 diabetes, Alzheimer disease, and skin hyperpigmentation. In addition, the antioxidantpotential of the extracts was also assessed using multiple methods. The detailed phytochemicalprofiles of the extracts were determined using high-performance liquid chromatography. Based onqualitative phytochemical fingerprint, a network pharmacology analysis was conducted as well.Parishin was identified from the water extract only, whereas gastrodin and caffeic acid derivativeswere present in the methanol extract. The methanol extract exhibited high inhibitory activityagainst tyrosinase (69.69 mg kojic acid equivalent/g extract), α-amylase (15.76 mg acarboseequivalent/g extract), and α-glucosidase (20.07 mg acarbose equivalent/g extract). Similarly, themethanol extract showed highest antioxidant potential (22.12, 44.23, 45.56, and 29.38 mg Troloxequivalent/g extract, for 2,2-diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), CUPric Reducing Antioxidant Capacity (CUPRAC),and Ferric Reducing Antioxidant Power (FRAP) assays, respectively). Finally, the results ofnetwork pharmacology analysis, besides corroborating traditional uses of plant extracts in themanagement of cold and flu, confirmed a direct involvement of identified phytochemicals in theobserved enzyme inhibitory effects, especially against tyrosinase, α-amylase, and α-glucosidase.Furthermore, based on the results of both colorimetric assays and network pharmacology analysis&nbsp;related to the activity of A. pyramidalis extracts and identified phytocompounds on enzymesinvolved in type 2 diabetes, a docking study was conducted in order to investigate the putativeinteractions of oxo-dihydroxy octadecenoic acid trihydroxy octadecenoic acid against aldosereductase, peroxisome proliferator-activated receptor (PPAR)-α, dipeptidyl peptidase (DPP)-IV,and α-glucosidase. Docking analysis suggested the inhibitory activity of these compounds againstthe aforementioned enzymes, with a better inhibitory profile shown by oxo-dihydroxyoctadecenoic acid. Overall, the present findings supported the rationale for the use of A. pyramidalis as source of bioactive metabolites and highlight, today more than ever, for the strongnecessity of linkage strategy between wild resource valorization and conservation policy.

The scientific world tends to turn to natural products such as medicinal and aromatic plants because of the inadequacy of commercially available synthetic drugs as antibiotics or anticancer, and their adverse effects on healthy tissues. One of these plants is Daphne gnidioides Jaub. & Spach, which belongs to the Thymelaeaceae family, and there is no data in the literature on its biological activity. This study is aimed to elucidate the chemical profiles and in vitro anticancer, antibacterial and DNA protection and enzyme inhibitory properties of methanol extracts of root, stem, and leaf of D. gnidioides Jaub. & Spach. Polyphenolic components of the extracts were characterized by HPLC-MS/MS. The highest phenolic content was detected in the leaf extract (TIPC = 43.5 ± 0.5 mg/g DE), followed by stem (TIPC = 27.3 ± 0.7 mg/g DE) and root (TIPC = 18.3 ± 0.2 mg/g DE) extracts. Vicenin-2 and 3-O-p-coumaroyl-5-O-caffeoylquinic acid were the main identified compounds in leaf and both root and stem extracts, respectively. The extracts did not show any protective effect on DNA against experimental Fenton's reagent. The minimum inhibitory concentration and the minimum bactericidal concentration values for the root and leaf extracts against tested bacterial strains ranged from 31.25 to 500 μg/mL. After 48 h interaction of the cancer cell lines with the extracts, only the stem extract had significant cytotoxicity on HeLa cells (IC 50 = 86.16 μg/mL). No remarkable activity of the extracts, which was tested against MDA-MB-231, was detected (IC 50 > 1000 μg/mL). These data showed that D. gnidioides Jaub. & Spach stem extract inhibited the survival of HeLa cells in a time-dependent manner. After the treatment of IC 50 concentration of stem extract with HeLa cells, an increase in LC3-II autophagic gene expression was detected. Also, the extracts exhibited significant tyrosinase inhibitory effects which were confirmed by molecular docking. To sum up, the tested extracts could be used as a starting point for the development of new multifunctional drugs., Competing Interests: Declaration of Competing Interest The authors declare no conflicts of interest., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

In this study, we attempted for the first time to determine the phytochemical compositions and biopharmaceutical properties of the methanolic and aqueous extracts of Morinda morindoides fruits and seeds. Antioxidant propensities of the extracts were determined via free radical-scavenging, phosphomolybdenum, metal chelating, and reducing power assays. Inhibitory activities against cholinesterases (acetylcholinesterase (AChE) and butyrylcholinesterase (BChE)), tyrosinase, α-amylase, and α-glucosidase were assessed. Moreover, the total phenolic and flavonoid contents were determined. High Performance Liquid Chromatography coupled to Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry (HPLC-ESI-Q-TOF-MS) analysis was performed to establish the chemical profile of the investigated extracts. The tested extracts showed remarkable antioxidant abilities with aqueous fruit extract being most potent in all assays, except for ferrous ion chelating assay. Overall, the methanolic extracts were potent inhibitors of the tested enzymes. In conclusion, M. morindoides may be endorsed as promising sources of bioactive compounds and used for designing functional foods. PRACTICAL APPLICATIONS: In recent years, new compounds from plant sources have attracted great interest to design functional foods. Thus, we aimed to detect biological and chemical properties of Morinda morindoides fruits and seeds, a widely used as food with medicinal properties in Africa. Based on our findings, fruits extracts exhibited stronger activity when compared to seed extracts. Also, chemical identification was performed for each extracts. The presented findings could provide valuable information into the pool of scientific knowledge and may be basis for the design of novel functional applications from M. morindoides., (© 2020 Wiley Periodicals, Inc.)

Broccolini is originated from crossing the regular broccoli with Chinese kale. Consequently, it has similar properties to these vegetables, but other very particular characteristics. Its consumption has increased in the last few years and, consequently, there have been some studies related to its quality parameters and the influence of different cooking methods. Nevertheless, changes on its phenolic composition and mineral content originated by its cooking have not been investigated in-depth so far. Here we report the phytochemical profile of broccolini before and after boiling, steaming, and griddling cooking treatments. The mineral content and phytochemicals were assessed by inductively coupled plasma-mass spectrometry (ICP-MS) and high performance liquid chromatography-mass spectrometry (HPLC-MS), respectively. The main phenolics (mainly hydroxycinnamic acid derivatives from caffeic, coumaric, ferulic and sinapic acids) were quantified. Three oxylipins, three flavonoid glycosides and the glucosinolate glucobrassicin were also identified. ABTS and DPPH assays were also used as screening methods to assess the antioxidant potential of broccolini. A significant loss of the phenolic compounds and a reduction of the antioxidant activity were observed after the three cooking methods. Clear disadvantages were detected when broccolini was boiled, namely high losses of phenolic acids and derivatives (70%). Steaming and griddling also led to a significant loss of phenolics (50%) from fresh broccolini. The mineral content of this vegetable after domestic cooking procedures is also reported for the first time, calculating the contribution of broccolini consumption to official daily recommendations., Competing Interests: Declaration of competing interest The authors declare no competing financial interest., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Cakile maritima Scop. (sea rocket) is an edible halophyte plant with several ethnomedicinal uses. This work reports the chemical profile and bioactivities of food grade extracts from sea rocket organs. Toxicity was determined on mammalian cells, and phenolic profiling and the quantitation of the main metabolites were made by high-performance liquid chromatography coupled to mass spectrometry (HPLC-MS). Enzymatic inhibition was determined towards acetyl- and butyrylcholinesterase (AChE, BuChE), α-glucosidase, α-amylase, and tyrosinase. Docking studies were performed to tyrosinase, on the major metabolites, and samples were tested for antioxidant properties. Extracts were not toxic, were constituted mainly by flavonoids, and some compounds (roseoside and oleuropein) are here described for the first time in the species. The aerial organs' ethanol extract had relevant activity towards 2,2-diphenyl-1-picrylhydrazyl [DPPH, half maximal inhibitory concentration (IC 50 ) = 0.59 mg/mL], and ferric-reducing activity power (FRAP, IC 50 = 0.99 mg/mL). All samples were more active towards AChE than on BuChE. The ethanol fruits' extract inhibited α-glucosidase [2.19 mmol of equivalent of acarbose (ACAE)/g]. Samples were active against tyrosinase, especially the aerial organs' ethanol extracts [25.9 mg of equivalent of kojic acid (KAE)/g]. Quercetin and kaempferol glycosides fit well into the enzymatic pocket of tyrosinase. Our results suggest sea rocket as a candidate to be further explored as a source of bioactive products., Competing Interests: The authors declare no conflict of interest.

Glyphosate (Gly) is the most widely used herbicide at the moment. It presents a broad spectrum of action, hence its use for many different crops. Regulatory agencies have constantly mentioned the low hazard potential of Gly to mammals. However, the International Agency for Research on Cancer concluded in 2015 that glyphosate is "probably carcinogenic to humans". For this reason, it is important to develop reliable analytical methods to quantify Gly in food samples. Here, we propose an analytical method that makes use of graphene quantum dots (GQDs) and cysteine-capped silver nanoparticles (AgNPs) for the screening of glyphosate, using QuEChERS as sample treatment. Gly quenched the luminescence of GQDs-AgNPs system, achieving an excellent sensitivity (detection limit of 9 ng mL -1 ) and selectivity. The method developed was applied to different types of pulses (peas and lupins), obtaining recoveries close to 100% and relative standard deviations lower than 4% in all cases. Its simplicity and rapidity make this method an interesting alternative to other existing methodologies for the analysis of this pesticide in food samples., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Packaging may represent a source of food contamination, as different organic compounds and degradation compounds may migrate from packaging to foodstuff. For fatty foods, rectified olive oil is the common simulant, which implies time-consuming and laborious liquid-liquid extraction (LLE) procedures to isolate the contaminant(s) from the oil. Here we propose a Multisyringe Flow Injection Analysis manifold to automate this sample treatment, using the monomer 4,4´-dihydroxybiphenyl as the contaminant. The LLE procedure, using water as extractant, was fully automated. After the on-line LLE, the resulting extract was pumped through a fluorescence detector, inside which a flow-cell filled with C 18 silica gel solid support was placed. The analyte was pre-concentrated on the solid support (in which the analytical signal was directly recorded), so improving the sensitivity of the system. Under optimum conditions, the method detection limit is 0.05 mg kg -1 , well within the specific migration limit of 6 mg kg -1 . The method developed was compared with the standard CEN test method (off-line LLE and HPLC determination) observing savings in sample and reagents of 90% and a 7-fold increase in sample throughput.

Pittosporum senacia (PS) Putt. (Pittosporaceae), indigenous to the Mascarene Islands, is a common ingredient in traditional medicines. However, there is currently a dearth of studies to validate some of these traditional claims. Given the broad traditional uses of PS against several diseases, we aimed to provide a comprehensive insight into the biological and chemical profile of P. senacia. The antioxidant, enzyme inhibitory activity, anticancer, and phytochemical composition of the methanolic extract of P. senacia leaf extracts were studied. The possible interaction and binding mode of the most abundant phytochemicals were studied via in silico docking experiments on tyrosinase and α-glucosidase. The mechanism behind the cytotoxic property of P. senacia extract for MDA-MB-231 was also examined using different methods including 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) cell viability test checking apoptosis-associated genes, and wound healing assays. Twenty-six compounds were identified, of which caffeoylquinic acid derivatives, ferulic acid derivative, cinnamoylquinic acid derivative and two other polyphenols (oleuropeine and isoramnetin glucoside) being abundant, have been tested using in silico studies, against α-glucosidase and tyrosinase. The extract (IC 50  = 118.8 μg/ml) exhibited time and dose dependent anti-proliferative effect on human breast cancer cell line, MDA-MB-231. According to the expression profile of apoptosis inhibitors and apoptosis promoters genes, expression of Bax and Bak genes were significantly increased compared to Bcl-2 and Birc5 genes. Based on wound healing analysis, cell migration was inhibited after the application of the plant extract. The present findings suggested that PS might be a good candidate as sources of bioactive compounds for designing functional applications., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

: Berberis species are known for their use in traditional medicine. Here, we report the phenolic composition and bioactivity of methanolic and aqueous extracts of Berberis thunbergii DC. leaves. The phenolic profiling and the quantitation of the main compounds were performed by high-performance liquid chromatography with diode array and mass spectrometry detections. The most abundant compounds in both extracts were caffeoylquinic acids (chlorogenic acid, particularly, with a concentration of 90.1-101.3 mg g - 1 dried extract), followed by caffeoylglucaric acids and quercetin glycosides. Antioxidant and radical scavenging assays (phosphomolybdenum, DPPH, ABTS, CUPRAC, FRAP, metal chelating activity), as well as enzyme inhibitory assays (acetylcholinesterase, butyrylcholinesterase, tyrosinase, amylase, glucosidase, and lipase), were carried out to evaluate the potential bioactivity of B. thunbergii . The methanolic extract presented the highest antioxidant and radical scavenging values, in agreement with its higher phenolic content. Regarding enzyme inhibitory potential, the methanolic extract was also more potent than the aqueous one. Hence, B. thunbergii leaves represent a suitable candidate for the preparation of pharmaceutical or nutraceutical products., Competing Interests: The authors declare no conflicts of interest.

Two methods for the luminescence determination of cysteine (Cys) are presented. They make use of either silver nanoparticles (Ag NPs) or graphene quantum dots (GQDs), both doped with terbium(III). The methods are based on the finding that Cys quenches the green luminescence of Tb(III)-Ag NPs and Tb(III)-GQDs. The excitation/emission maxima are at 306/545 and 257/545 nm, for both nanoprobes, respectively. Response is linear in the 0.28-5.0 μg mL -1 Cys concentration range for the Tb(III)-Ag NP system, and from 0.05-3.0 μg mL -1 for the Tb(III)-GQD system. The respective limits of detection are 0.09 and 0.015 μg mL -1 . The probes were applied to the time-resolved luminometric determination of Cys in (spiked) food supplements and gave satisfactory results. Graphical abstractSchematic representation of the quenching by cysteine (Cys) of the time-resolved luminescence (TSL) of terbium-graphene quantum dots [Tb(III)-GQD] and of terbium-silver nanoparticles [Tb(III)-Ag NP].

In this work, we present an automated luminescence sensor for the quantitation of the insecticide thiacloprid, one of the main neonicotinoids, in lettuce samples. A simple and automated manifold was constructed, using multicommutated solenoid valves to handle all solutions. The analyte was online irradiated with UV light to produce a highly fluorescent photoproduct (λ exc /λ em = 305/370 nm/nm) that was then retained on a solid support placed in the flow cell. In this way, the pre-concentration of the photoproduct was achieved in the detection area, increasing the sensitivity of the analytical method. A method-detection limit of 0.24 mg kg -1 was achieved in real samples, fulfilling the Maximum Residue Limit (MRL) of The European Union for thiacloprid in lettuce (1 mg kg -1 ). A sample throughput of eight samples per hour was obtained. Recovery experiments were carried out at values close to the MRL, obtaining recovery yields close to 100% and relative standard deviations lower than 5%. Hence, this method would be suitable for routine analyses in quality control, as an alternative to other existing methods.

The main goals of this study were to determine the phenolic composition and antioxidant activity of table olives from Olea europaea L. cv. Cornezuelo, as well as the effect caused by a simulated in vitro digestion to evaluate compounds bioavailability. High-performance liquid chromatography with diode-array and mass spectrometry detection (HPLC-DAD-MS n ) was used to evaluate the phytochemical profile, whereas conventional spectrophotometric methods (ABTS· + and DPPH) were used to determine the antioxidant activity. The mineral content was also quantified by inductively coupled plasma - mass spectrometry. Thirty compounds were identified, mainly polyphenols, quantifying the major compounds by HPLC-DAD. After the simulated digestion, the phenolic content suffered an important decrease - more than 50% - reaching losses of up to 75% for oleuropein and comselogoside isomers. This decrease also resulted in a loss of antioxidant activity, observing significant differences for all parameters. However, the analyzed extracts still retained considerable antioxidant potential., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Africa is famous for its floral biodiversity, exploited by local people for therapeutic purposes. However, such plants need to be scrutinised scientifically for the presence of bioactive compounds and possible biological properties. This study attempts for the first time to highlight the pharmacological and phytochemical profile of extracts prepared from leaves and stem barks of three African plants (Macaranga hurifolia Beille, Sterculia tragacantha Lindl. and Zanthoxylum gilletii (De Wild.) P. G. Waterman. The extracts were tested for antioxidant and enzyme inhibitory effects. Free radical scavenging, metal chelator, reducing power and phosphomolybdenum assays were performed to evaluate antioxidant effects. To identify enzyme inhibitory effects, cholinesterases (acetylcholinesterase (AChE) and butrylcholinesterase (BChE)), tyrosinase, α-amylase and α-glucosidase were selected as target enzymes. High performance liquid chromatography-Electrospray tandem mass spectrometry (HPLC-ESI-MS) technique was also used for chemical profiling. ABTS (2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) and DPPH (1,1-diphenyl-2-picrylhydrazyl) radical scavenging assays showed that the stem barks of all three African plants were better scavenger than leaf extracts. Sterculia tragacantha was found to be a better metal chelator (64.10 ± 4.66 mg EDTAE/g) among the studied plants. All extracts exhibited good clinical enzyme inhibitory activities. The stem bark of S. tragacantha exhibited the best acetylcholinesterase activity compared to the other plants. HPLC-ESI-MS characterization showed that the most abundant compounds in stem bark were flavonoids in M. hurifolia (4.2 ± 0.2 mg/g DE), proanthocyanidins in S. tragacantha (42 ± 1 mg/g DE) and similar concentrations of phenolic acids and flavonoids in Z. gilletii (2.8-3.1 mg/g DE). Based on the biological activity, the most abundant and relevant bioactive compounds in the extracts were studied using molecular modelling approach against tyrosinase. The studied African plants showed good antioxidant and enzymatic propensities and thus can be considered as potential bioresources for future development of nutraceuticals and/or for pharmaceutical applications., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Ethnobotanical evidences substantiate the use of several Centaurea species to treat and/or manage several human ailments. In the present study, the phytochemical profile of the ethyl acetate, methanol, and aqueous extracts (prepared by infusion and decoction) of Centaurea bornmuelleri Hausskn. aerial parts was established. The enzyme inhibitory and antioxidant properties were also determined by in vitro bioassays. Methanol extract (38.58 mg gallic acid equivalent/g extract) and ethyl acetate extract (38.83 mg rutin equivalent/g extract) possessed the highest concentration of phenolics and flavonoids, respectively. Aqueous extract prepared following traditional infusion method showed potent DPPH (38.54 mg TE/g extract) and ABTS (57.75 mg TE/g extract) scavenging abilities. The methanol extract (101.46 mg TE/g extract) of C. bornmuelleri exhibited potent reducing activity in the CUPRAC assay while the aqueous extract obtained by infusion was more active in the FRAP assay (69.81 mg TE/g extract). Ethyl acetate extract of C. bornmuelleri inhibited both acetylcholinesterase (1.14 mg galantamine equivalent [GALAE]/g extract), butyrylcholinesterase (0.63 mg GALAE/g extract), tyrosinase (69.84 mg kojic acid equivalent/g extract), amylase (19.90 mg acarbose equivalent [ACAE]/g extract), and glucosidase (33.12 mg ACAE/g extract). The phytochemical profile of C. bornmuelleri has been characterized and the main components quantified in order to provide scientific base to design innovative products including pharmaceuticals, cosmetics or nutraceuticals although further investigation concerning the isolation of the main bioactive compounds would be required., (Copyright © 2019 Elsevier B.V. All rights reserved.)

In this work, the phenolic composition of E. umbellata leaves and berries is reported. Berries were rich in flavonols, whereas leaves presented abundant flavonols and ellagitannins. Then, the enzyme-inhibitory properties, anti-glycation and antioxidant activities of E. umbellata and Sambucus lanceolata (its phenolic profile has been already established in a previous work) were tested by several in vitro assays and compared. The simulated gastrointestinal digestion resulted in a decrease on their phenolic composition. Nevertheless, both species still had the ability to inhibit aldose reductase activity and protein glycation and scavenge free radicals at the end of the process. Thus, the potential beneficial effects of E. umbellata and S. lanceolata seems to be kept to some extent after passage throughout the digestive system. Altogether, this study provides further insight into investigation of these species as dietary sources of bioactive compounds to lower the risk of type-2 diabetes and obesity., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Consumption of herbal teas, infusions and other plant-related products has always been popular due to the related health benefits. However, the safety of these products needs to be assessed, for example monitoring the potential presence of contaminants such as pesticides. In this paper, we report an analytical method for determining three neonicotinoid insecticides - thiacloprid, thiamethoxam, and imidacloprid - that are widely used worldwide. This method is based on quenching by analytes of the luminescence signal of terbium ions. Terbium presents a time-resolved luminescence signal at 256/545 nm/nm, which is quenched by the presence of low concentrations of the selected analytes. Detection limits of 0.1, 0.2 or 0.75 μg ml -1 were obtained for thiamethoxam, thiacloprid and imidacloprid, respectively. Recovery experiments in different teas (green tea, black tea, chamomile, peppermint) were performed at concentrations lower than the maximum residue limits established by the European Union and the Codex Alimentarius for tea samples. In all cases, satisfactory recovery yields were observed, and the results were compared with a chromatographic reference method. The proposed method therefore proved suitable for quantifying these insecticides, fulfilling the current legislation., (© 2019 John Wiley & Sons, Ltd.)

In order to value J. glutinosa DC (rock tea), we characterised its phenolic profile and antioxidant activity. The study was performed in aqueous extracts before and after a simulated in vitro digestion to obtain data regarding phenolics bioavailability. Methanolic extracts were also analysed for comparison purposes. Phytochemical profiles were determined by high-performance liquid chromatography with mass spectrometric detection, whereas total phenolic content (TPC) and antioxidant assays were performed by conventional spectrophotometric methods. The most abundant compounds were dicaffeoylquinic acids, representing more than 90% of phenolics in tea infusions. Statistically significant differences were observed for all parameters except for TPC in methanol and aqueous extracts. Both phenolics amount and antioxidant activities were lower after the in vitro digestion of the infusions. However, although phenolics were lost during the simulated digestion, rock tea is still a good source of bioactive compounds with potential applications in the pharmaceutical or nutraceutical industries., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

This study attempts to compare the pharmaceutical potential (antioxidant and key enzyme inhibition of clinical relevance) of organic and aqueous extracts of Parentucellia latifolia (L.) Caruel subsp. latifolia (L.) Caruel as well as phytochemical composition. The phytochemical compounds were evaluated by spectrophotometric methods (for total amounts) and HPLC-ESI-DAD-MS n (for individual compounds). The extracts were screened for antioxidant abilities by in vitro assays. Inhibition effects were also investigated against a set of enzymes linked to major health problems. Generally, the methanol (MeOH) and aqueous extracts displayed higher scavenging abilities on radicals and reductive effects when compared with the ethyl acetate (EtOAc) extract. On the other hand, the EtOAc extract was the most active inhibitor on cholinesterases (1.81-1.88 mg GALAE/g), amylase (0.70 mmol ACAE/g), glucosidase (2.85 mmol ACAE/g) and lipase (33.24 mg OE/g). The highest TPC was observed in the aqueous extract (25.07 mg GAE/g) while MeOH extract possessed the highest level of TFC (44.15 mg RE/g) and TPAC (3.46 mg CE/g). LC-MS n metabolite profiling indicated that loganin and its isomers, rutin, and luteolin-O-hexoside were the most abundant compounds. Our results suggest that P. latifolia may be valuable source of phyto-agents for the management of noncommunicable diseases., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Myrica faya Aiton (fire tree, faya) is an underused species with a diverse flavonoid composition (anthocyanins, flavonols, ellagitannins) which can promote positive effects on human health. M. faya has been reported to possess high antioxidant activities, but its potential in the prevention of type II diabetes has not been evaluated so far. In the present study, eight M. faya samples from different areas of Madeira and Azores archipelagos (Portugal) were collected to determine their phytochemical profile and then tested for their in vitro anti-diabetic and antioxidant activities. The analyzed extracts showed strong inhibitory activities towards α -glucosidase, aldose reductase and glycation of bovine serum albumin (BSA) and moderate effects towards α-amylase and lipase (by comparison with reference compounds). Cyanidin-3-O-glucoside and ellagitannins were the main bioactive agents involved in the anti-diabetic effects of M. faya. Such results may provide important scientific evidence for further utilization of M. faya as dietary or nutraceutical products for the prevention and/or control of hyperglycaemia-associated complications., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Objectives: This study investigates into the biological effects of solvent extracts (ethyl acetate, methanol, and water) of Scutellaria orientalis L. and Scutellaria salviifolia Benth. based on its enzyme inhibitory activity and antioxidant ability together with the screening of bioactive compounds., Methods: Total and individual bioactive components were determined using spectrophotometric and HPLC-ESI-MS methods. Six antioxidant assays were conducted and enzyme inhibition was tested against key enzymes linked to the pathology of common chronic disorders., Key Findings: Results revealed that the aqueous extracts of both plants exerted better 2,2'-azino-bis(3-ethylbenzothiazoline)-6-sulfonic acid scavenging, reducing power, metal chelating, and α-glucosidase inhibitory activities. The methanol extracts showed highest tyrosinase inhibition and antioxidant activity in phosphomolybdenum assay while the less polar ethyl acetate extracts showed better acetylcholinesterase, butyrylcholinesterase, and α-amylase inhibition. Phytochemical evaluation by HPLC-ESI-MS revealed the presence of high amounts of flavones., Conclusions: Scutellaria orientalis and S. salviifolia are important sources of bioactive agents that warrants further studies., (© 2018 Royal Pharmaceutical Society.)

Phyllanthus phillyreifolius var. commersonii Müll. Arg is an endemic plant of Mauritius. To date, no study has been performed concerning its polyphenolic profile and pharmacological properties. In this study, a decoction (water), ethyl acetate and methanol extracts of the aerial parts of P. phillyreifolius, obtained from different extraction procedures (maceration and Soxhlet), were studied for antibacterial, antioxidant, anticancer, and enzyme inhibitory properties along with their polyphenolic profile. The ethyl acetate macerated extract showed high antibacterial activity against B. cereus (MIC = 0.293 mg/mL) and E. coli (MIC = 0.417 mg/mL) while S. epidermidis was most susceptible to the ethyl acetate-Soxhlet extract (MIC = 0.521 mg/mL). The methanol-Soxhlet extract displayed the most potent cupric and ferric reducing power, and metal chelating effect, while the macerated methanolic extract was the most effective DPPH and ABTS scavenger, and BChE inhibitor. Only the ethyl acetate-Soxhlet extract exhibited α-glucosidase inhibition. All extracts exhibited a strong anti-tyrosinase activity, which was further investigated by molecular docking and molecular dynamic. After 48 h exposure to the extracts for HeLa cell lines, the ethyl acetate-Soxhlet extract showed the highest inhibition (IC 50  = 533.1 μg/mL) while the decoction extract was more cytotoxic to MDA-MB-231 cells (IC 50  = 337.4 μg/mL). Treatment of cancer cell lines with all P. phillyreifolius extracts resulted in a time-dependent reduction of cell viability for HeLa and dose-and time-dependent reduction for MDA-MB-231. Gene expression ratio of Bcl-2 to Bax was higher for all Soxhlet-extracts. Total phenolics (TPC) and flavonoids (TFC) content were highest in the decoction and methanol-Soxhlet extract, respectively (122.43 mg GAE/g extract and 31.28 mg RE/g extract, respectively). The extracts were abundant in ellagitannins, although phenolic acids and flavonoids were also detected. Granatin B was detected for the first time in Phyllanthus species. Overall, the aerial parts of P. phillyreifolius exemplify a potent reservoir of bioactive phytochemicals for therapeutic applications., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Rubus grandifolius Lowe (wild blackberries) is an endemic species from Madeira Archipelago (Portugal) used in folk medicine for alleviating diabetic complications. In this work, R. grandifolius methanolic extracts were analysed for in vitro inhibitory effect on digestive enzymes linked to type-2 diabetes, as well as aldose reductase activity and protein glycation. The phenolic composition, antioxidant and cytotoxic activities were also determined. Methanolic extracts exhibited strong inhibition of glucosidases (α- and β), but were less potent for α-amylase and pancreatic lipase when compared to current pharmaceutical drugs. The total phenolic content determined by HPLC-DAD varied between 92.96 - 97.47 and 118.01-137.41 mg g -1 of dry extract for berries and leaves, respectively. Fifty polyphenols were quantified, anthocyanins and ellagitannins being the main compounds. Cyanidin-3-glucoside was identified as one of the main hypoglycaemic and hypolipidemic agents in all extracts. R. grandifolius also prevented glycation of bovine-serum albumin (BSA) and showed strong radical scavenging activity against tested free radicals. At low concentration, the extracts were not cytotoxic against Caco-2 cells. Based on the results of this study, wild blackberry extracts demonstrated a potential beneficial effect on the control/management of type-2 diabetes mellitus, validating their use in folk medicine., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Zearalenone (ZEA), a mycotoxin produced by several Fusarium molds, can be found in many cereals and related products. The toxicity of ZEA has been reported for both humans and animals. Therefore, many countries have adopted regulations in foods and feed materials to limit the exposure to this contaminant. In this paper, we propose a multicommutated flow-through optosensor to quantify ZEA in different cereal samples. ZEA was retained and pre-concentrated on C 18 silica gel, and the use of the multicommutated flow manifold allowed the automated retention/desorption of ZEA on the solid microbeads by the use of appropriate carrier/eluting solutions, hence increasing the selectivity and sensitivity of the system. The native fluorescence of ZEA was recorded on the solid phase at λ exc /λ em of 265/465 nm/nm. A QuEChERS procedure was used to carry out the extraction of ZEA from different cereal samples (feedstuff materials). Recovery studies were performed to assess the accuracy of the method, obtaining recovery yields between 93% and 107% in all the analyzed samples. LC-MS was employed as reference method. The quantitation limit of the proposed method was low enough to fulfill the maximum residue levels established by the Commission of the European Communities, thus demonstrating its potential use for the analysis of ZEA in feedstuffs., (Copyright © 2018 Elsevier B.V. All rights reserved.)

In this work, we report the phytochemical profile and antioxidant activity of different morphological parts of Rumex maderensis Lowe (Polygonaceae), a wild leafy-vegetable growing in Madeira Island (Portugal). Methanol extracts from leaves, flowers, and stems were submitted to high-performance liquid chromatography with mass spectrometry detection to obtain the phytochemical profile, which allowed the identification of 86 polyphenols (about 70% C- and O-flavonoids) and 9 non-phenolic compounds. In vitro antioxidant activities were measured against ABTS, DPPH, nitric oxide and superoxide free radicals. Then, the samples were subjected to an in vitro digestion, observing a decrease of about 50% in both the content of phenolics and the antioxidant activity. However, relevant antioxidant capacity was still observed after the simulated digestion. Therefore, this study supports the consumption of R. maderensis as an interesting foodstuff and a dietary source of antioxidant phytochemicals that survive the gastrointestinal digestion process., (Copyright © 2018 Elsevier Ltd. All rights reserved.)