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Lignans are polyphenolic compounds that are considered phytoestrogens for their plant origins, and they possess different biological activities. Three different extraction methods, ie, "dilute and shoot", acidic hydrolysis, and enzymatic digestion, have been compared for extracting lignans (secoisolariciresinol (SECO), matairesinol (MAT), and lariciresinol (LARI)) from espresso coffee (EC) by using high-performance liquid chromatography (HPLC) tandem mass spectrometry (MS/MS). The best recovery values (SECO: 97%, LARI: 98%, and MAT: 93%) were obtained by using enzymatic hydrolysis with Clara-Diastase at 10% (w/v), keeping the sample at 37°C for 3 hours. For this reason, this method has been chosen and then applied to quantify lignans in 9 different EC samples from 5 different geographical origins (Brazil, Colombia, El Salvador, Ethiopia, and India). Secoisolariciresinol and LARI were found in all EC samples from 27.9 to 52.0 μg L -1 and from 5.3 to 27.8 μg L -1 respectively, contrary to MAT that it was not possible to detect it in each type of coffee. This method confirms the high specificity and sensitivity of MS/MS system for detecting bioactives in complex matrix such as coffee., (© 2018 John Wiley & Sons, Ltd.)

Consumption of legumes has become popular among health-conscious consumers due to the high levels of nutrients such as proteins, dietary fibres, minerals, vitamins and micronutrients like polyphenols. Ten legumes cultivars organically and conventionally grown were compared regarding their chemical profiles in terms of total phenolic content (TPC), total anthocyanin content (TAC), total flavonoid content (TFC) and their antioxidant capacity. The chemical profiles (i.e. free phenolics and anthocyanins) were determined with aid of new high-performance liquid chromatography-diode array detection (HPLC-DAD) method able to identify two individual anthocyanins and 15 polyphenols. Results showed that phenolic acids, namely gallic acid, caffeic acid, syringic acid and ferulic acid, are mainly significantly higher in the organic samples with respect to the conventional ones. All organic legumes showed a higher antioxidant capacity with respect to conventional samples with the exception of red and yellow dehulled lentils.

(+)-Cyclazosin [(+)-1] is one of most selective antagonists of the α 1B -adrenoceptor subtype (selectivity ratios, α 1B /α 1A  = 13, α 1B /α 1D  = 38-39). To improve the selectivity, we synthesized and pharmacologically studied the blocking activity against α 1 -adrenoceptors of several homochiral analogues of (+)-cyclazosin featuring different substituents on the carbonyl or amine groups, namely (-)-2, (+)-3, (-)-4-(-)-8, (+)-9. Moreover, we studied the activity of some their opposite enantiomers, namely (-)-1, (-)-3, (+)-6, and (-)-9, to evaluate the influence of stereochemistry on selectivity. The benzyloxycarbonyl and methyl (4aS,8aR) analogues (+)-3 and (-)-6 improved in a significant way the α 1B selectivity of the progenitor compound: 4 and 14 time vs. the α 1D subtype and 35 and 77 times vs. the α 1A subtype, respectively. The study confirmed the importance of the hydrophobic cis-octahydroquinoxaline moiety of these molecules for the establishment of interactions with the α 1 -adrenoceptors as well that of their (4aS,8aR) stereochemistry to grant selectivity for the α 1B subtype. Hypotheses on the mode of interaction of these compounds were advanced on the basis of molecular modeling studies performed on compound (+)-3., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) are priority contaminants that bioaccumulate through the food webs and affect the biology of a variety of resident and migratory species, including sea turtles. Few studies have evaluated toxicological biomarkers of exposure to PAHs and PCBs in these animals. The present paper reports the results of an initial field study to quantify the association between plasma concentrations of PAHs/PCBs and whole blood cell expression of gene biomarkers in juvenile loggerhead sea turtles (Caretta caretta) rescued along the Italian coasts of the northern and central areas of the Adriatic Sea. While detectable levels of PAHs were found in all plasma samples examined, only three PCB congeners (PCB52, PCB95, and PCB149) were noted, with detection percentages ranging between 48% and 57%. A significant correlation was found between 3 of the 6 gene biomarkers assessed (HSP60, CYP1A and ERα) and plasma levels of some PAH congeners. In contrast, no significant association between PCB burden and gene expression was observed. The global DNA methylation levels were significantly and positively correlated with the concentrations of most of the PAHs and only one of the PCB congeners (PCB52). The relation between PAH concentration and gene expression in whole blood cells suggests that these genes may respond to environmental contaminant exposure and are promising candidates for the development of biomarkers for monitoring sea turtle exposure to persistent organic pollutants (POPs)., (Copyright © 2017 Elsevier B.V. All rights reserved.)

The aim of the study was to identify new potential chemical markers of extra virgin olive oil (EVOO) quality by using a multicomponent analysis approach. Sixty-six EVOOs were purchased from the Italian market and classified according to their price as low price EVOOs (LEVOOs) and high price EVOOs (HEVOOs) costing 3.60-5.90euro/L and 7.49-29.80euro/L respectively. Sensory and chemical parameters strictly related to olive oil quality have been investigated, like volatile substances, polar phenolic substances, antioxidant activity, fatty acid composition, and α-tocopherol. Significant differences in terms of chemical composition and sensory features have been highlighted between the two EVOOs classes investigated, proving a generally lower level of quality of LEVOOs, clearly showed also by means of principal component analysis. Among the most interesting outcomes, R ratio (free tyrosol and hydroxytyrosol over total free and bound forms), measuring the extent of secoiridoids hydrolysis, resulted to be significantly higher in LEVOOs than in HEVOOs. Other key differences were found in the volatile substances composition, in the stearic acid percentage and in p-coumaric acid content., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Scope: The aim of our work was to produce a hydroalcoholic extract of lentils and to examine (a) the hypocholesterolemic action in an animal model, by studying the plasma cholesterol level and the concentration of bile acids in the feces; (b) the potential prebiotic effect, by conducting an in vitro culture fermentation experiment and assessing the level of SCFAs in the feces of rats., Methods and Results: Lentil extract (LE) was obtained by extracting lentils with a solution of H 2 0/EtOH (70/30 v/v) for 3 h, and the content of main nutrients was determined. After 71 days of diet-induced hypercholesterolemia in rats, LE reduced the cholesterol level of rats of 16.8% (p < 0.05) and increased the level of bile acids in the feces of rats (p < 0.01). LE revealed the same prebiotic activity of inulin and good bifidogenic activity, inasmuch as it enhanced the growth of Bifidobacterium spp. by 3 log (p < 0.05). The concentration of SCFAs in the feces of rats fed with LE increased during the time of the study., Conclusion: This new hydroalcoholic extract obtained from lentils was shown to possess hypocholesterolemic and prebiotic properties, and could have interesting applications in the field of nutraceuticals., (© 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Rosemary essential oil (REO) contains bioactives having antioxidant and antimicrobial properties. This work investigated the effect of REO combined with modified atmosphere packaging conditions (MAP), in our case, aerobic, vacuum or high O 2 , to extend the shelf life of beef. Beef slices were wrapped in special three-layer sheets of packaging material, some with a coating of REO (active packaging, AP), and some without REO (non active packaging, NAP), and stored at 4°C for 20days. The use of REO proved efficacious in every storage condition, as seen in the lower counts of psychrotrophics, Brochothrix thermosphacta, Pseudomonas spp., and Enterobacteriaceae in AP meat compared to NAP meat. Sensory and colourimetric analyses showed that the best packaging conditions were high-O 2 atmosphere in combination with REO. Based on microbiological data, shelf life of beef was 5-6days for AP samples packaged under aerobic conditions and 14-15days for AP samples in high-O 2 conditions., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Pulses, which include lentils, beans, chickpeas, peas, and soybeans, provide an important source of proteins, dietary fibers, minerals and vitamins, as well as such important bioactive molecules as polyphenols. The presence of polyphenols is often related to the colour of the pulse and to its antioxidant activity. The aim of this work was to set up a new HPLC-DAD method for simultaneously analysing 14 polyphenolic compounds, including two anthocyanins, in different varieties of pulses and to correlate the polyphenol content with the seed coat colour and the antioxidant activity. The total content of the analysed polyphenols ranged from 3mg/kg for dehulled red lentils to 1630.5mg/kg for ruviotto beans. Samples with dark testa (or seed coat), namely black lentils and diavoli beans, had higher antioxidant activity than those with pale testa, and a positive correlation was found between total phenolic content (TPC) and IC 50 for dark coloured varieties., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Schizogyne sericea, well-known as 'salado', is a halophytic shrub widespread on coastal rocks of Tenerife (Canary Islands). This plant is used traditionally as analgesic, astringent, anti-inflammatory and vulnerary agent. In the present work, we have analysed the aqueous and ethanolic extracts of S. sericea for the content of phenolic acids by HPLC-DAD. The dynamic solid-liquid Naviglio® extractor was used to extract the flowering aerial parts. Aqueous extracts showed higher levels of phenolics than ethanolic extracts. S. sericea extracts were rich in chlorogenic and isochlorogenic acids. The Naviglio® extracts obtained were assayed for in vitro biological activities, namely antioxidant, antimicrobial and cytotoxicity on tumour cells by DPPH, ABTS, FRAP, agar disc-diffusion and MTT methods, respectively. Results showed that aqueous extracts, being richer in phenolic acids, are endowed with relevant radical scavenging activity (TEAC values in the range 208-960 μmol TE/g) while ethanolic extracts exhibited noteworthy antiproliferative effects on tumour cells.

Rosmarinus eriocalyx is an aromatic evergreen bush endemic to Algeria where it is used as a condiment to flavour soups and meat and as a traditional remedy. In the present work we have analyzed for the first time the phenolic composition of polar extracts obtained from stems, leaves and flowers of R. eriocalyx by HPLC, and determined the antioxidant and antimicrobial effects by DPPH, ABTS, FRAP, ORAC and agar disc diffusion methods, respectively. Results showed that ethanolic extracts of leaves and flowers are a rich source of phenolic compounds, mainly rosmarinic acid, carnosic acid and carnosol that are the main responsible for the noteworthy antioxidant activity observed in the assays. This study showed that R. eriocalyx might be a spice to be included in the European food additive list and used as a preservative agent besides R. officinalis., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Recent evidences suggest that the toxicological effects of endocrine disrupting chemicals (EDCs) involve multiple nuclear receptor-mediated pathways, including estrogen receptor (ER) and peroxisome proliferator-activated receptor (PPAR) signaling systems. Thus, our objective in this study was to detect the summated endocrine effects of EDCs with metabolic activity in coastal waters of the central Adriatic Sea by means of a toxicogenomic approach using seabream hepatocytes. Gene expression patterns were also correlated with seawater levels of polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs). We found that seawater extracts taken at certain areas induced gene expression profiles of ERα/vitellogenin, PPARα/Stearoyl-CoA desaturase 1A, cytochrome P4501A (CYP1A) and metallothionein. These increased levels of biomarkers responses correlated with spatial distribution of PAHs/PCBs concentrations observed by chemical analysis in the different study areas. Collectively, our data give a snapshot of the presence of complex EDC mixtures that are able to perturb metabolic signaling in coastal marine waters., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

In order to assess if an extra virgin olive oil (EVOO) can be acknowledged with the health claim related to olive oil polyphenols (Reg. EU n.432/2012), a new method to quantify these species in EVOO, by means of liquid-liquid extraction followed by HPLC-DAD/MS/MS of the hydroalcoholic extract, has been developed and validated. Different extraction procedures, different types of reverse-phase analytical columns (Synergi Polar, Spherisorb ODS2 and Kinetex) and eluents have been tested. The chromatographic column Synergi Polar (250×4.6mm, 4μm), never used before in this kind of application, provided the best results, with water and methanol/isopropanol (9/1) as eluents. The method allows the quantification of the phenolic alcohols tyrosol and hydroxytyrosol, the phenolic acids vanillic, p-coumaric and ferulic acids, secoiridoids derivatives, the lignans, pinoresinol and acetoxypinoresinol and the flavonoids luteolin and apigenin. The new method has been applied to 20 commercial EVOOs belonging to two different price range categories (3.78-5.80 euros/L and 9.5-25.80 euros/L) and 5 olive oils. The obtained results highlight that acetoxypinoresinol, ferulic acid, vanillic acid and the total non secoiridoid phenolic substances resulted to be significantly higher in HEVOOs than in LEVOOs (P=0.0026, 0.0217, 0.0092, 0.0003 respectively). For most of the samples analysed there is excellent agreement between the results obtained by applying the HPLC method adopted by the International Olive Council and the results obtained by applying the presented HPLC method. Results obtained by HPLC methods have been also compared with the ones obtained by the colorimetric Folin-Ciocalteu method., (Copyright © 2016 Elsevier B.V. All rights reserved.)

A new, fast and simple analytical method that is able to identify and quantify simultaneously 17 steroid hormones and metabolites (pregnenolone, 17-OH-pregnenolone, progesterone, 17-OH-progesterone, androsterone, androstenedione, dehydroepiandrosterone, dehydroepiandrosterone sulfate, testosterone, cortisol, corticosterone, aldosterone, 11-deoxycortisol, 11-deoxycorticosterone, dihydrotestosterone, estrone and estradiol) has been developed in equine serum using the ultra-high-performance liquid chromatography-tandem mass spectrometry technique. A total of 400 µl of sample was deproteinized with 1000 µl of acetonitrile, evaporated, restored with 50 µl of a solution of 25% methanol and injected in ultra-high-performance liquid chromatography-tandem mass spectrometry triple quadrupole. The recovery percentage obtained by spiking the matrix at two different concentrations with a standard mixture of steroid hormones was in all cases higher than 85.60% and with the percentage of coefficient of variation lower than 8.37%. The range of the correlation coefficients of the calibration curves of the analyzed compounds was 0.9922-0.9986, and the limits of detection and limits of quantification were in the range of 0.002-2 and 0.0055-5.5 ng ml -1 , respectively. The detected limit of quantification for testosterone (i.e. 50 pg ml -1 ) is twofold lower with respect to its threshold admitted in geldings plasma (100 pg ml -1 free testosterone). The high sensitivity and the quantitative aspect of the method permitted to detect most of the steroids in equine serum. Once validated, the method was used to quantify 17 steroid hormones in mare, stallion and gelding serum samples. The main steroids detected were corticosterone (range 37.25-51.26 ng ml -1 ) and cortisol (range 32.57-52.24 ng ml -1 ), followed by 17-OH-pregnenolone, dihydrotestosterone and pregnenolone. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

A new method for extracting isoflavones from espresso coffee (EC) was coupled with high-performance liquid chromatography-tandem mass spectrometry (MS/MS) for the first time to analyse five isoflavones, which included both a glycosilated form, genistin and the aglycons daidzein, genistein, formononetin and biochanin A. Isoflavones were extracted from coffee samples using methanol, stored in a freezer overnight to precipitate proteic or lipidic residues and purified on SPE C18 cartridges before high-performance liquid chromatography-MS/MS analysis. The recovery percentages obtained by spiking the matrix at concentrations of 10 and 100 µg l(-1) with a standard mixture of isoflavones were in the range of 70 to 104%. The limits of detection and limits of quantification were in the range of 0.015-0.3 µg l(-1) and 0.05-1 µg l(-1) , respectively. Once validated, the method was used to analyze the concentrations of isoflavones in six ECs and ten ground coffee samples. Only formononetin and biochanin A were found, and their respective concentrations ranged from 0.36 to 0.41 µg l(-1) and from 0.58 to 3.26 µg l(-1) in ECs and from 0.36 to 4.27 µg kg(-1) and from 0.71 to 3.95 µg kg(-1) in ground coffees. This method confirms the high specificity and selectivity of MS/MS systems for detecting bioactives in complex matrices such as coffee.Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Analysis of the complex composition of cocoa beans provides fundamental information for evaluating the quality and nutritional aspects of cocoa-based food products, nutraceuticals and supplements. Cameroon, the world's fourth largest producer of cocoa, has been defined as "Africa in miniature" because of the variety it habitats. In order to evaluate the nutritional characteristics of cocoa beans from five different regions of Cameroon, we studied their polyphenolic content, volatile compounds and fatty acids composition. The High Performance Thin Layer Chromatography (HPTLC) analysis showed that the Mbalmayo sample had the highest content of theobromine (11.6 mg/g) and caffeic acid (2.1 mg/g), while the Sanchou sample had the highest level of (-)-epicatechin (142.9 mg/g). Concerning fatty acids, the lowest level of stearic acid was found in the Mbalmayo sample while the Bertoua sample showed the highest content of oleic acid. Thus, we confirmed that geographical origin influences the quality and nutritional characteristics of cocoa from these regions of Cameroon.

In the present work we conducted a comprehensive chemical analysis of blue honeysuckle (Lonicera caerulea) spontaneously growing in eastern Russia. HPLC-DAD-ESI/MS analysis showed cyanidin-3-glucoside as the major constituent among phenolics, while nutritional analysis revealed fibre, protein, calcium and magnesium as the most important macro- and micronutrients, respectively. Fatty acid composition was dominated by polyunsaturated fatty acids, linoleic acid being the most abundant. Furthermore, we evaluated several in vitro biological activities such as antioxidant, antimicrobial, antiproliferative, wound healing and immunomodulatory effects of blue honeysuckle aqueous and ethanolic extracts that are often incorporated in food and nutraceutical preparations. While the fruit extracts were revealed to be potent radical scavengers with significant inhibition of ABTS radical, thus confirming the literature data, their inhibitory effects against microbial pathogens and tumor cell lines were negligible. The fruit aqueous extract did not show toxicity to human fibroblasts, but 24 h treatment with 150-200 μg per mL of extract slightly enhanced the cell migration when tested by scratched wound assay. Worth mentioning was the inhibitory effect displayed by the blue honeysuckle fruit aqueous extract on human lymphocytes.

Hypericum androsaemum, also known as Tutsan, is a small evergreen shrub common in the Mediterranean basin where it is traditionally used as diuretic and hepatoprotective herbal drug. This plant possesses the peculiarity to produce fleshy and berry-like fruits that ripen from red to shiny black. In the present work, the chemical constituents of methanolic extracts and infusions of red and black fruits were analyzed by HPLC, and correlated with their antioxidant properties which were evaluated by the DPPH, β-Carotene/linoleic acid, and hypochlorous acid tests. In addition, the red pigment of the fruit was isolated by column chromatography and structurally elucidated by NMR. Results showed that H. androsaemum fruits contain high amounts of shikimic and chlorogenic acids, while their color was given by a tetraoxygenated-type xanthone, reported for the first time in Hypericum species. The red berries infusion gave the highest content of total phenolic compounds, DPPH, and hypochlorous acid scavenging activity, and β-carotene bleaching. Cytotoxicity of the berries extracts on three human tumor cell lines (malignant melanoma, breast adenocarcinoma, and colon carcinoma) was evaluated by MTT assay, and relevant inhibition on colon carcinoma cells (IC50 value of 8.4 μg/mL) was found. Finally, the effects of red berries extract on the immune system were evaluated by peripheral blood mononuclear cell (PBMC) proliferation assay that revealed a strong stimulation on lymphocytes at low doses (0.4-6 μg/mL).

This study sought to contribute to the assessment of the nutritional properties of legumes by determining the fatty acid (FA) composition of 29 legume samples after the evaluation of nine extraction methods. The Folch method and liquid-solid extraction with hexane/isopropanol or with hexane/acetone were investigated, as was the effect of previous hydration of samples. Soxhlet extractions were also evaluated with different solvent mixtures. Results on FA composition using the hexane/isopropanol extraction method were the same in terms of FA composition of the Folch method, but the extraction yield was only around 20-40% of that of the Folch method preceded by hydration. Some types of legumes showed particularly interesting values for the ratio of polyunsaturated fatty acids (PUFAs) n-6/n-3, such as lentils, with the value of 4.0, and Azuki beans, at 3.2. In lentils, the PUFAs% ranged from 42.0% to 57.4%, while in Azuki beans it was 57.5%., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Tolerance to opioid administration represents a serious medical alert in different chronic conditions. This study compares the effects of the imidazoline compounds 1, 2, and 3 on morphine tolerance in an animal model of inflammatory pain in the rat. 1, 2, and 3 have been selected in that, although bearing a common scaffold, preferentially bind to α2-adrenoceptors, imidazoline I2 receptors, or both systems, respectively. Such compounds have been tested in vivo by measuring the paw withdrawal threshold to mechanical pressure after complete Freund's adjuvant injection. To determine the ligand levels in rat plasma, an HPLC-mass spectrometry method has been developed. All the compounds significantly reduced the induction of morphine tolerance, showing different potency and duration of action. Indeed, the selective imidazoline I2 receptor interaction (2) restored the analgesic response by maintaining the same time-dependent profile observed after a single morphine administration. Differently, the selective α2C-adrenoceptor activation (1) or the combination between α2C-adrenoceptor activation and imidazoline I2 receptor engagement (3) promoted a change in the temporal profile of morphine analgesia by maintaining a mild but long lasting analgesic effect. Interestingly, the kinetics of compounds in rat plasma supported the pharmacodynamic data. Therefore, this study highlights that both peculiar biological profile and bioavailability of such ligands complement each other to modulate the reduction of morphine tolerance. Based on these observations, 1-3 can be considered useful leads in the design of new drugs able to turn off the undesired tolerance induced by opioids., (Copyright © 2015 Elsevier B.V. All rights reserved.)

The root of Gentiana lutea L., famous for its bitter properties, is often used in alcoholic bitter beverages, food products and traditional medicine to stimulate the appetite and improve digestion. This study presents a new, fast, and accurate HPLC method using HPLC/ESI-MS and HPLC/DAD for simultaneous analysis of iridoids (loganic acid), secoiridoids (gentiopicroside, sweroside, swertiamarin, amarogentin) and xanthones (isogentisin) in different populations of G.lutea L., cultivated in the Monti Sibillini National Park, obtained wild there, or purchased commercially. Comparison of HPLC/ESI-MS and HPLC/DAD indicated that HPLC/ESI-MS is more sensitive, reliable and selective. Analysis of twenty samples showed that gentiopicroside is the most dominant compound (1.85-3.97%), followed by loganic acid (0.11-1.30%), isogentisin (0.03-0.48%), sweroside (0.05-0.35%), swertiamarin (0.08-0.30%), and amarogentin (0.01-0.07%). The results confirmed the high quality of the G.lutea cultivated in the Monti Sibillini National Park., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Legumes are an excellent source of macronutrients and phytochemicals as isoflavones. The aim of this work was to develop a new analytical method for determining five isoflavone compounds, three of which are aglycons, namely daidzein, genistein, biochanin A, and two of which, daidzin and genistin, are glycosilated, in lentils and other pulses, using an effective clean-up system and UHPLC-MS/MS (triple quadrupole) method. The recoveries obtained by spiking the lentil samples with a standard mixture of isoflavones at three levels of fortification (5, 25 and 100 μg kg(-1)) were in the range of 54.4-111.1%, 68.6-91.1%, and 84.4-114%, respectively. The method was applied to analyse 48 lentil samples from central Italy and pulses for determining the isoflavone content, which was found to range from 1.1 to 95.6 μg kg(-1)., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Alternariol (AOH) is a mycotoxin produced by Alternaria spp. Soyasaponin I (Ss-I) is present naturally in legumes, and it has antioxidant properties. Cytotoxic and genotoxic effects of AOH have been demonstrated previously in vitro. In the present study, the cytotoxicity of AOH, Ss-I, and soyasaponins-rich extract from lentils was investigated; as well as, the cytoprotective effects of Ss-I and lentil extracts against AOH induced-cytotoxicity on Caco-2 cells. Cytotoxicity was carried out using MTT and PC assays (AOH: 3.125-100 µM, Ss-I: 3.125-50 µM, and lentil extracts: 1:0-1:32) during 24 h of exposure. Only AOH showed cytotoxic effect. The reduction in cell proliferation ranged from 25% to 47%. Simultaneous combination of Ss-I with AOH (1:1) increased cell proliferation (35%) compared to AOH tested alone. The Ss-I and extracts showed synergistic cytoprotective effects against cytotoxicity induced by AOH on Caco-2 cells. Food commodities containing Ss-I could contribute to diminish the toxicological risk that natural contaminant as AOH in diet can produce to humans., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

In the present work we carried out a phytochemical and biological investigation on three Hypericum species, i.e. Hypericum reflexum, Hypericum canariense and Hypericum grandifolium, from the Canary Islands where they are traditionally used as diuretic, wound healing, vermifuge, sedative and antidepressive agents. The polar extracts of the top flowering aerial parts, prepared by Soxhlet apparatus using a methanol-acetone (1:1) extracting mixture, were analyzed by HPLC-DAD and HPLC-MS for the content of eight biomarkers such as hypericin, hyperforin, chlorogenic acid, rutin, hyperoside, isoquercitrin, quercitrin and quercetin, whereas the hydrodistilled essential oils were analyzed by GC-FID and GC-MS. The three Hypericum species had different results in both polar and volatile constituents, H. reflexum being the only one endowed with a small amount of naphtodianthrones (hypericin and pseudohypericin), and containing high levels of chlorogenic acid, rutin and volatile mono- and sesquiterpenes. After chemical characterization, all products were in vitro biologically assayed for antiproliferative activity on human tumor cell lines by MTT assay, for antioxidant potential by DPPH, ABTS and FRAP assays, and for antimicrobial activity by the agar disc diffusion and microdilution methods. Results revealed interesting bioactivities and differences between polar extracts and essential oils, with the former being endowed with significant antioxidant activity and the latter with comparable inhibition effects on the tumor cells (A375, MDA-MB 231 and HCT 116) to that of cisplatin., (Copyright © 2014 Elsevier B.V. All rights reserved.)

Coffee is one of the most popular hot drinks in the world; it may be prepared by several methods, but the most common forms are boiled (brew) and pressurized (espresso). Analytical studies on the substances responsible for the pleasant aroma of roasted coffee have been carried out for more than 100 years. Brew coffee and espresso coffee (EC) have a different and peculiar aroma profile, demonstrating the importance of the brewing process on the final product sensorial quality. Concerning bioactive compounds, the extraction mechanism plays a crucial role. The differences in the composition of coffee brew in chlorogenic acids and caffeine content is the result of the different procedures of coffee preparation. The aim of the present review is to detail how the brewing process affects coffee aroma and composition.

Background: Poncirus trifoliata, also known as trifoliate orange, is a tree native to China and Korea and widely used all over the world as a rootstock breeding material. In this study the differences among the volatile profiles of flavedo, pulp and seeds from two cultivars (var. trifoliata and var. monstrosa) grown in Italy (Marche, Abruzzo and Sicily) were determined. Headspace solid phase microextraction and hydrodistillation techniques were used in combination with GC/FID and GC/MS to obtain the volatile profiles of the samples., Results: Both techniques permitted the differentiation of fruit parts based on the main volatile components: the flavedo was characterized by monoterpene hydrocarbons such as limonene and myrcene, the seeds were characterized by sesquiterpene hydrocarbons such as (E)-caryophyllene and germacrene D, while the pulp showed an intermediate composition. The main differences in volatile profiles obtained by the two techniques were analyzed by chemometric techniques such as principal component analysis., Conclusion: The study did not highlight significant differences in volatiles between the two cultivars of trifoliate orange, while few differences in the number of volatiles in the fruit parts were revealed by the two techniques., (© 2014 Society of Chemical Industry.)

In this work, we present for the first time a rapid and robust UHPLC-MS/MS method for analyzing taurine, GlcLA and GlcA in energy drinks simultaneously and without derivatization. The separation of three analytes was achieved using a Kinetex Hilic analytical column (100 mm × 4.6 mm i.d.) and a mobile phase formed by water (A) and acetonitrile (B) both with formic acid 0.1% at a flow rate of 0.8 ml min(-1) with isocratic elution in 3.5 min. Calibration curves were calculated using the method of standard addition in a concentration range from 2 to 6 mg/100 ml for taurine (R(2)>0.987), from 0.4 to 1.2 mg/100 ml for GlcLa (R(2)>0.997), and from 0.2 to 0.6 mg/100 ml for GlcA acid (R(2)>0.998). The validated method was applied to the analysis of nine commercial energy drinks. The level of taurine found ranged from 0.01 to 0.45 g/100 ml, and it matched with that reported in the labels of the analyzed energy drink samples., (Copyright © 2014 Elsevier B.V. All rights reserved.)

Biogenic amines (BAs) are considered to be important indicators of freshness and quality in food. In this work, an analytical method for analyzing ten underivatized BAs in meat by performance liquid chromatography-tandem mass spectrometry has been developed. Comparison between ion trap and triple quadrupole as mass analyzers indicated that the latter provides greater sensitivity and selectivity. The range of the correlation coefficients of the calibration curves of the analyzed compounds was 0.987-0.999, and the limits of detection and limits of quantification were in the range of 0.002-0.1 mg l(-1) and 0.008-0.5 mg l(-1), respectively. Once validated, the method was used to analyze the concentrations of BAs in 16 commercial meat samples, for evaluating the freshness of food through the study of BA indices, i.e. biogenic amine index (BAI) and the ratio spermidine/spermine (SPD/SPE). The results indicated that all the samples were fresh, with a BAI lower than 1.49 mg kg(-1) and a SPD/SPE ratio lower than 0.41 in each case. This methodology for testing the freshness of meat has potential for quality control applications along the entire production chain of meat products., (Copyright © 2014 John Wiley & Sons, Ltd.)

Caffeine, trigonelline and nicotinic acid are important bioactive constituents of coffee. In this work, the combination of different water temperatures and pressures in the settings of the espresso coffee (EC) machine was evaluated, to assess how these factors influence how effectively caffeine, trigonelline and nicotinic acid are extracted from both Arabica and Robusta samples. The proposed analytical method, based on a high performance liquid chromatography (HPLC) system coupled to a variable wavelength detector (VWD), showed good linearity (R²> 0.9985) and good recoveries (71-92%); after validation for three monitored compounds, the method was used to analyze 20 commercial samples. The combination of a temperature of 92 °C and pressure at 7 or 9 bar seems to be the ideal setting for the most efficient extraction of these compounds and consequently for their intake; the compound extracted in the greatest quantity was caffeine, which was in the range of 116.87-199.68 mg in a 25 ml cup of coffee.

Solid-phase microextraction technique coupled with gas chromatography-flame ionisation detector and gas chromatography-mass spectrometry was used to investigate the inter- and intra-population chemical polymorphism in volatile constituents of three populations of Thymus pannonicus growing in Slovakia. To have an idea on what really the plant emits under different environmental and physiological conditions, a total of 86 individuals were separately analysed using low extraction temperatures (30°C). Data were analysed using a chemometric approach such as the principal component analysis which revealed a significant intra-population variability with the existence of up to four chemotypes: the most abundant is the p-cymene/γ-terpinene chemotype, followed by the geraniol and linalool chemotypes, and, only in one population, by the γ-muurolene/(E)-caryophyllene chemotype. This differentiation of individual plants inside the populations allows better adaptation to ecological conditions of localities and is probably connected with intrinsic genetic diversity of the species.

Biogenic amines (BAs) are considered as an important indicator of freshness and quality of food. In this work, a new active packaging (AP) system for meat that, incorporating essential oil of Rosmarinus officinalis at 4% (w/w), inhibits the increase of BAs and the bacteria involved into their production was developed. BAs were analyzed by a SPE-HPLC-DAD method during the storage time of meat (0-7 d, 4 °C). Results showed that, in each monitored day, Biogenic Amine Index (BAI) expressed in mg kg(-1) is lower in meat wrapped in AP with respect to that packed in polycoupled packaging (PP) (from 19% to 62%). A strong correlation was found between the inhibition of increase of putrescine, cadaverine, histamine and their bacteria producers such as Enterobacteriaceae, Pseudomonas spp. and Brocothrix thermospacta. By exploiting antimicrobial and antioxidant action of essential oil of R. officinalis, the new APs contribute to increase the shelf life of fresh meat and to preserve its important nutrients.

Smyrnium olusatrum, better known as Alexanders or wild celery, is a biennal herb used in cuisine for many centuries by Romans in many dishes, where it has now been replaced by celery. In order to provide additional evidences so that this forgotten vegetable can be reconsidered in the human diet, as well as in pharmaceutics, the essential oils obtained from different parts and its main isolated furanosesquiterpenes were in vitro biologically assayed for antiproliferative activity on human tumor cell lines by MTT assay, for antioxidant potential by DPPH, ABTS and FRAP assays, and for antimicrobial activity by the agar disc diffusion method. The essential oils showed cytotoxic effects on tested human tumor cell lines, related to the furanosesquiterpenoid content; the IC(50) values on colon carcinoma, glioblastoma, and breast adenocarcinoma cells were 8.51, 13.35, and 14.81 μg/ml, respectively. Isofuranodiene and 1β-acetoxyfuranoeudesm-4(15)-ene resulted the most active constituents. The essential oils possessed also radical scavenging activity., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Pharmacological effects of hydroalcoholic extract prepared from Hypericum origanifolium Willd. (Guttiferae) on behavioral parameters and pain perceptions of mice were investigated in this study. Depression, anxiety, spontaneous locomotor activity, and motor coordination parameters of mice were assessed by modified forced swimming, hole board, activity cage, and rota-rod tests, respectively. In addition, antinociceptive effect was evaluated by performing hot-plate, tail-clip, and formalin tests. Reboxetine (20 mg/kg), diazepam (1 mg/kg), and morphine (10 mg/kg) were used as reference antidepressant, anxiolytic, and analgesic drugs, respectively. Phytochemical analyses exhibited that chlorogenic acid (2317.12 ppm) and rutin (2108.79 ppm) were the main phenolic compounds in the H. origanifolium extract. The extract (50, 100, and 250 mg/kg) induced significant antidepressant, anxiolytic, and antinociceptive activities following the acute administrations. Anxiolytic effect was antagonized by flumazenil (a benzodiazepine receptor antagonist, 2.5 mg/kg, i.p.) pre-treatment, which indicated the participation of GABA(A)-benzodiazepine receptor complex in the activity. Moreover, centrally and peripherally mediated antinociception reversed by naloxone (a non-selective opioid receptor antagonist, 5 mg/kg, i.p.) pre-treatment, indicating the involvement of opioid system in the pharmacological action. These findings are the first to indicate the pharmacological effects of the H. origanifolium extract on the emotional state and pain perceptions of mice., (Copyright © 2012 John Wiley & Sons, Ltd.)

Legumes contain a rich variety of phytochemicals as soyasaponins, triterpenoidal glycosides that possess multiple health-promoting properties, such as lowering of cholesterol. In this work, the quantification of soyasaponins I and βg in 60 raw and cooked legumes by using a solid phase extraction (SPE) coupled to a liquid chromatography (LC)-mass spectrometry (MS) method was carried out. Results showed that lentils are a good source of soyasaponins, with a content of soyasaponin I that ranged from 636 to 735 mg kg(-1) and of soyasaponin βg from 672 to 1807 mg kg(-1). The cooking process produced a small loss of soyasaponins in water, that is, 4.8-8.7%, and partially converted soyasaponin βg into soyasaponin I. In addition, the bioaccessibility of soyasaponins I in lentils was studied; the values ranged from 8.9 ± 0.3 to 10.6 ± 1.1% in the duodenal compartment. On the basis of these results, soyasaponins could be effective in lowering exogenous cholesterol.

This study was undertaken to assess the antioxidant and antiproliferative potential of the essential oil of Hypericum hircinum L. subsp. majus (Aiton) N. Robson. Analysis of the oil composition revealed that sesquiterpene hydrocarbons (69.3%) dominate, cis-β-guaiene, δ-selinene and (E)-caryophyllene being the most representative. Significant values of antioxidant activity were found using 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS) radical scavenging assays. The essential oil revealed antiproliferative activity as evaluated on human glioblastoma (T98G), human prostatic adenocarcinoma (PC3), human squamous carcinoma (A431) and mouse melanoma (B16-F1) tumour cell lines by MTT assay.

Smyrnium olusatrum, well known as wild celery or Alexanders, is a biennial herb belonging to the Apiaceae and used for many centuries as an edible vegetable because of the aromatic flavour of its parts. Its use on the table has decreased since the Middle Ages when it was replaced by common celery (Apium graveolens). In the present work the composition of the essential oils obtained by hydrodistillation of various plant parts was investigated by gas chromatography (GC-FID and GC-MS), while quantitation of a heat-sensitive compound, isofuranodiene, known for its anticancer activity, and of its Cope rearrangement product curzerene, was achieved by HPLC-DAD. All essential oils were composed mainly of furanosesquiterpenoids (54.1-76.2%) with isofuranodiene (19.5-45.8%) as the main constituent. Results showed that GC analysis provides underestimation (up to five times) of isofuranodiene levels in essential oils and that curzerene could be considered an artifact since it is produced during heating of plant material, occurring during hydrodistillation., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

The aroma profile and the final quality of espresso coffee (EC) are influenced by such technical conditions as the EC machine extraction temperature and the pressure used. The effect of these two parameters on EC quality were studied in combination by headspace solid phase micro extraction-gas chromatography-mass spectrometry (SPME-GC-MS) and sensory profile. Moreover, 10 key odorants at the best EC machine settings were examined to compare the two coffee cultivars (Arabica and Robusta) and two EC machines [Aurelia Competizione (A) and Leva Arduino (B)]. The data obtained provides important information about espresso making technique, suggesting that the usual espresso machine temperature and pressure settings (i.e. 92°C and 9bar) are very close to those needed to obtain the best quality espresso. This confirms the traditional wisdom of coffee making, which judges 25ml, the typical volume of a certified Italian EC, to be ideal for very strong aroma intensity., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Enniatins (ENs) are bioactive compounds produced by the secondary metabolism of several Fusarium strains and are known to have various biological activities, such as acting as enzyme inhibitors, antifungal antibacterial agents, and immunomodulatory substances. This study investigated the bioaccessibility of the ENs in wheat crispy breads produced with three different inulin concentrations (1, 5 and 10%). The mean bioaccessibility data of the four ENs (A, A(1), B and B(1)) ranged from 68.67% to 84.67 in the experiments carried out without inulin, whereas the data ranged from 51.00 to 74.00% in the experiments carried out with the wheat crispy bread produced with 5 and 10% of the inulin.

Montepulciano is one of the most famous and important red-berried grapes of Italy. This article presents and discusses a comparative study of aroma profile and phenolic content of the Montepulciano wine from the Marches and the Abruzzo regions. The volatile composition of wines was determined by using headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). The PDMS fibre was chosen. The dominating esters in Montepulciano wines were ethyl hexanoate, ethyl decanoate, and ethyl octanoate, whereas phenyl ethanol and 3-methyl-1-butanol were dominating alcohols. Phenolic compounds, namely gallic acid, p-coumaric acid, trans-ferulic acid, caffeic acid, trans-resveratrol, (+)-catechin and (-)-epicatechin, were examined using HPLC-MS with direct injection of wine samples. The total phenolic content of the analysed wines was in the range of 30.4-61.9mgl -1 . The presence of high amounts of esters seems to characterise the volatiles of Montepulciano wines from the Marches, whereas a high level of alcohols was found in Montepulciano wines from Abruzzo. Moreover, multivariate chemometric techniques, such as cluster analysis and principal component analysis, supported this thesis. Headspace solid phase microextraction and gas chromatography-mass spectrometry were used to analyse 20 commercial wine samples (Montepulciano monovarietal red wines) from the Marches (10 samples) and Abruzzo (10 samples)., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

The aim of this study was to verify the effectiveness of Achillea ligustica essential oils against several oral microorganisms in comparison with a commercial essential oil-containing mouthrinse (Listerine(®)) and clove oil (containing 89% eugenol). The inhibition efficacy of A. ligustica essential oils alone and in combination with Listerine(®) was evaluated by the micro-dilution method. The most susceptible microorganisms were Bacillus cereus, Streptococcus pyogenes, and Candida albicans. The efficacy was similar to that of the clove oil. The antiseptic mouthwash Listerine(®) did not exert a strong inhibition on microbial strains tested, whereas its effectiveness increased significantly when essential oil was added. The study provides additional evidence for the in vitro inhibitory activity of A. ligustica essential oils on several pathogens, suggesting their usefulness in mouthrinse formulations as an adjunct to mechanical oral hygiene regimens. Essential oil-containing mouthrinses can be beneficial, safe components of daily oral health routines, representing an efficient and without side effect alternative to prevent and control oral infections., (Copyright © 2012 Verlag Helvetica Chimica Acta AG, Zürich.)

In this study, a headspace solid-phase microextraction (HS-SPME) method, in combination with gas chromatography flame ionisation detector and gas chromatography-mass spectrometry, has been developed for use in the analysis of the volatile compounds of Teucrium flavum L. subsp. flavum, a plant whose particular fragrance is used in the preparation of flavoured wines, bitters and liqueurs, or as a substitute for hops in the flavouring of beer. The tested fibres were 100 µm poly(dimethylsiloxane) (PDMS), the 65 µm PDMS/divinylbenzene (DVB) and 50/30 µm DVB-carboxen-PDMS. The best fibre was found to be PDMS when working in the following conditions: 60°C temperature, 30 min extraction time, 30 mg sample amount, 1 mm sample particle size. The HS-SPME method permitted the identification (95.8-97.8%) of 76 (dry) and 66 (fresh) different volatiles. In addition, we discovered that the presence of water in the sample can enhance the absolute quantity of alcoholic compounds such as 1-octen-3-ol and reduce the presence of esters such as methyl geranate.

Sideritis italica (Mill.) Greuter et Burdet belongs to the Lamiaceae family and is endemic to Italy. The glandular trichomes (morphology, distribution, histochemistry, and ultrastructure) of the plant were studied for the first time, along with the chemical composition of the essential oils. Abundant non-glandular hairs and peltate (type A) and capitate (types B, C(1), and C(x)) glandular trichomes were observed both on the vegetative and reproductive organs. The histochemical procedures and the ultrastructural investigation enabled specific location of the main site of essential oil production mainly in type-A peltate hairs. Particular emphasis is given to the release mechanism of the secreted material in all of the types of glands, and the potential taxonomic value of the indumentum in the Lamiaceae family is briefly discussed. Essential oils were hydrodistilled from flowering aerial parts of S. italica, and 136 compounds (112 in flowerheads, 79 in vegetative parts) were identified. The quantitative prevalence of diterpenoids (43.4% in flowerheads and 22.3% in vegetative parts) was the most significant characteristic of the essential oil of S. italica that could be classified as a diterpene-rich essential oil according to the classification of Kirimer., (Copyright © 2011 Verlag Helvetica Chimica Acta AG, Zürich.)

The aim of this work was to trap the volatiles released from whole frozen and dry aerial parts, and, separately, from different organs (leaves, stems, corolla and calyx) of bastard balm (Melittis melissophyllum L., Lamiaceae) populations collected in Italy and Slovakia by HS-SPME, and to identify the headspace constituents responsible for the characteristic aroma impression by GC/FID and GC/MS techniques. Among more than 100 volatile components detected, the C(8) alcohol oct-1-en-3-ol, responsible for the typical mushroom-like odor, and the phenolic coumarin, with a characteristic sweet and creamy vanilla bean odor, played a major role in the aroma of whole aerial parts and different plant organ samples. In particular, dry calyx parts could be proposed as flavoring agent in food products as mushroom aroma enhancer. Multivariate chemometric techniques, such as cluster analysis and principal component analysis, were used to characterize the sample populations according to the geographical origin and processing of plant material., (Copyright © 2011 Verlag Helvetica Chimica Acta AG, Zürich.)

This study was designed to investigate possible antidepressant-like effects of the extract prepared from the flowers of Hypericum montbretti Spach. (Guttiferae, Clusiaceae). Phytochemical constituents of the methanolic extract were analysed by HPLC method. The main flavonoid component was detected as rutin, and another highly concentrated phenolic compound was quercitrin. Antidepressant activity of the extract was examined by tail suspension and modified forced swimming tests, whereas the motor coordination of the animals was tested by the Rota-Rod apparatus. Reboxetine at a dose of 20  mg kg⁻¹ was used as a reference drug. Dose-dependent antidepressant activity was observed in both tests following the administration of extract at 100 and 250 mg kg⁻¹ doses. To the best of our knowledge, this is the first study reporting the antidepressant activity of H. montbretti extract. Additionally, the results of this work support previous papers reporting the antidepressant activity of rutin.

This present study was undertaken to examine treating effects of St. John's Wort (SJW) extract on nociceptive perception of STZ-diabetic animals based on its potential antidiabetic and antinociceptive activities. One week administrations of SJW extract (125 and 250 mg/kg) induced significant decrease in high blood glucose levels of three weeks STZ-diabetic rats and improved their dysregulated metabolic parameters. In addition, SJW extract treatment caused restoration in the mechanical hyperalgesia of diabetic animals. These findings provide a rationale for the traditional use of SJW against diabetes and display the potential of this plant as a new drug candidate/source for the treatment of diabetic pain., (Copyright © 2011 Elsevier B.V. All rights reserved.)

Melittis melissophyllum (Lamiaceae) is a perennial herb, typical of woody places, occurring in Italy with two subspecies, i.e., melissophyllum and albida. So far, the classification of these two taxa was only based on morphology, i.e., the presence of glandular trichomes, the dimension of the leaves, and the number of teeth on each side as the main discriminant characters. To find marker compounds to chemically discriminate the subsp. melissophyllum with respect to the subsp. albida, a solid-phase microextraction SPME analysis coupled with GC/FID (=flame ionization detector) and GC/MS was carried out. SPME proved to be a chemotaxonomically useful technique that permitted a clearly differentiation of the two subspecies at headspace level. The subsp. melissophyllum was characterized by high amount of the mushroom alcohol oct-1-en-3-ol and the phenolic coumarin, whilst the subsp. albida exhibited a high content in monoterpenes and sesquiterpenes, α-pinene, sabinene, and (E)-caryophyllene being the major compounds. Multivariate chemometric techniques, such as cluster analysis (CA) and principal-component analysis (PCA), were used to support chemical data and characterize the population according to the taxonomy. In addition, the micromorphology and distribution of glandular trichomes of both subspecies were studied by scanning electron microscopy (SEM)., (Copyright © 2011 Verlag Helvetica Chimica Acta AG, Zürich.)

For centuries, Hypericum perforatum has been used in folk medicine to treat wounds. In the present study, the wound healing activities of extracts of H. perforatum ssp. perforatum (HPP) and H. perforatum ssp. veronense (HPV) were evaluated by comparing with a titrated extract of Centella asiatica (TECA) on NIH3T3 fibroblasts. The cells were incubated with the extracts. Using microscopical methods by staining cells, mitotic ability, morphological changes and collagen production in the fibroblasts were evaluated as parameters to approach possible wound repair mechanism(s). The wound healing activity caused an increase in the percentage of polygonal fibroblasts and in collagen granule numbers in fibroblasts of HPP and HPV. At 1 µg/mL, HPP caused a greater increase in mitotic cell numbers than HPV. The most increases in polygonal cell numbers were observed with HPV at 1 and 10 µg/mL. The number of collagen granules was increased with 1 µg/mL HPV being higher than HPP. As an indication of cytotoxic effects, round cells in response to HPV and HPP extracts, were found to be increased in concentrations higher than 10-50 µg/mL. The results indicated that the two subspecies of H. perforatum have different wound healing profiles as a result of the fibroblast migration and stimulation of collagen synthesis., (Copyright © 2010 John Wiley & Sons, Ltd.)

Headspace solid-phase microextraction (HS-SPME) coupled with GC/FID and GC/MS was applied for the first time in the analysis of the volatile fraction of an Ephedra species. Notably, six Italian populations (Marche, Abruzzo, and Sardinia) of Ephedra nebrodensis subsp. nebrodensis, covering almost the entire Italian area, were investigated to examine the chemical variability and to support the taxonomy of the species. A fiber screening with polymethylsiloxane (PDMS), Carboxen(TM) /polymethylsiloxane (CAR/PDMS), and polymethylsiloxane/divinylbenzene (PDMS/DVB) coatings, together with an optimization of the extraction conditions were carried out before analysis of the six populations. A total of 119 volatiles were identified in the headspace of different samples, accounting for 63.35-100.00% of the total volatiles. A great variability was found in the qualitative composition of different samples, since only 18 components were in common among all populations. The headspace composition was dominated by sesquiterpene hydrocarbons (52.30-88.32%), with β-maaliene (traces-7.49%), β-patchoulene (traces-1.29%), β-panasinsene (traces-6.85%), α-isocomene (traces-31.25%), α-trans-bergamotene (traces-6.95%), alloaromadendrene (traces-33.20%), α-acoradiene (traces-9.41%), and γ-muurolene (0.61-16.33%) being the most abundant constituents. Noteworthy is the occurrence in a sample of two major unknown sesquiterpenes, one hydrocarbon (24.49%, RI: 1396) and one oxygenated compound (10.37%, RI: 1591), whose mass spectra were reported for the first time. Multivariate chemometric techniques, such as cluster analysis (CA) and principal component analysis (PCA), were used to characterize the samples according to the geographical origin., (Copyright © 2011 Verlag Helvetica Chimica Acta AG, Zürich.)

Evidence shows that the endocannabinoid system modulates the addictive properties of nicotine. In the present study, we hypothesized that spontaneous withdrawal resulting from removal of chronically implanted transdermal nicotine patches is regulated by the endocannabinoid system. A 7-day nicotine dependence procedure (5.2 mg/rat/day) elicited occurrence of reliable nicotine abstinence symptoms in Wistar rats. Somatic and affective withdrawal signs were observed at 16 and 34 hours following removal of nicotine patches, respectively. Further behavioral manifestations including decrease in locomotor activity and increased weight gain also occurred during withdrawal. Expression of spontaneous nicotine withdrawal was accompanied by fluctuation in levels of the endocannabinoid anandamide (AEA) in several brain structures including the amygdala, the hippocampus, the hypothalamus and the prefrontal cortex. Conversely, levels of 2-arachidonoyl-sn-glycerol were not significantly altered. Pharmacological inhibition of fatty acid amide hydrolase (FAAH), the enzyme responsible for the intracellular degradation of AEA, by URB597 (0.1 and 0.3 mg/kg, i.p.), reduced withdrawal-induced anxiety as assessed by the elevated plus maze test and the shock-probe defensive burying paradigm, but did not prevent the occurrence of somatic signs. Together, the results indicate that pharmacological strategies aimed at enhancing endocannabinoid signaling may offer therapeutic advantages to treat the negative affective state produced by nicotine withdrawal, which is critical for the maintenance of tobacco use.

Tamsulosin (-)-1 is the most utilized α(1)-adrenoceptor antagonist in the benign prostatic hyperplasia therapy owing to its uroselective antagonism and capability in relieving both obstructive and irritative lower urinary tract symptoms. Here we report the synthesis and pharmacological study of the homochiral (-)-1 analogues (-)-2-(-)-5, bearing definite modifications in the 2-substituted phenoxyethylamino group in order to evaluate their influence on the affinity profile for α(1)-adrenoceptor subtypes. The benzyl analogue (-)-3, displaying a preferential antagonist profile for α1A-than α1D-and α1B-adrenoceptors, and a 12-fold higher potency at α1A-adrenoceptors with respect to the α1B subtype, may have improved uroselectivity compared to (-)-1., (Copyright © 2010 Elsevier Masson SAS. All rights reserved.)

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) was used in this study to obtain protein fingerprints of seven different lentil varieties, to characterize their differences and similarities. Two different matrices have been tested in order to obtain reproducible and significant mass spectra. Extraction with water containing 0.1% of trifluoroacetic acid has been used as preparative step to obtain hydrophilic protein samples of lentil seeds. The obtained MALDI protein profiles identified clear differences between the seven studied lentil varieties. Moreover, considering the high complexity of the obtained MALDI spectra, multivariate techniques of data analysis were employed to find further classification details. These multivariate analyses confirmed the possibility of a clear classification of the seven lentil varieties, indicating that the proposed procedure can be a valid taxonomic tool, and a method to certify the origin of lentils, useful for high added value lentils (Italian lentils)., (Copyright © 2010 John Wiley & Sons, Ltd.)