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Essential oils obtained by hydrodistillation of leaves (LV), flowers (FL) and fruits (FR) of Hypericum hircinum subsp. majus from Marche (Italy), were analyzed by gas chromatography-flame ionization detector (GC-FID) and gas chromatography/mass spectrometry (GC/MS). Ninety-two volatile components were identified in the oils, representing 81.41-94.36% of the total oils. The major compounds were cis-β-guaiene (23.25-41.23%) and δ-selinene (8.48-25.20%) in LV, δ-selinene (18.29%) and limonene (15.23%) in FL, limonene (14.01-38.72%) and β-pinene (9.88-16.31%) in FR. The oils from LV and FL were dominated by sesquiterpene hydrocarbons, whilst the FR oils were rich in monoterpenes. Seasonal changes in relative percentages of representative groups and compounds of the oils were discussed. [ABSTRACT FROM AUTHOR]

Abstract: Coumarin occurs in many plants used as flavoring and is known to possess hepatotoxic effects. Despite in the EFSA ‘Compendium of botanicals containing toxic substances’ coumarin is reported to be present in Melittis melissophyllum (bastard balm), a plant traditionally used as beverage in Italy and Serbia, to the best of our knowledge quantitative data has never been reported. Thus, the amount of coumarin in bastard balm leaves and its variation during the annual phenological cycle were determined. The subsp. melissophyllum resulted to contain high levels of coumarin (14,392mg/kg), mainly in the early stages of the plant cycle, suggesting prudence in its use as beverage. Furthermore, coumarin was found to be useful as marker compound to differentiate the bastard balm subspecies occurring in Italy, since the subsp. albida contained a much lower content of this molecule (19–34mg/kg). [Copyright &y& Elsevier]

Abstract: Ferula glauca L. (Apiaceae), formerly believed a subspecies of Ferula communis L., but at the present considered a distinguishable species, was studied for the first time for volatiles from leaves, flowers, fruits and roots. The chemical analysis of the essential oil obtained from different populations growing in Marche (central Italy) was performed by GC-FID and GC–MS. The differences in composition detected between F. glauca and F. communis made the volatile fraction a reliable marker to distinguish between them, and confirmed the botanical data at the base of their discrimination. In particular, the oils obtained from leaves and roots, contained as major compounds (E)-caryophyllene, caryophyllene oxide, myristicin and elemicin, that can be useful as marker components. Finally, the oils contained some daucane derivatives, that were detected also in F. communis and responsible for important biological properties. [Copyright &y& Elsevier]

Ready-to-eat (RTE) and ready-to-heat (RTH) dishes are food items that help save time, physical energy, and mental effort in all food-related activities. Convenience of use, variability of supply, and adaptability to different consumption occasions have led to an increase of acceptance among consumers through the years. Specialized databases can help in this context, where food composition databases can provide information and data to create sustainable nutritional models by reducing the now growing number of chronic diseases. This paper aims at developing a database of LanguaL TM and FoodEx2 codes of 50 food preparations and ready-to-eat dishes designed for consumption outside the home. LanguaL TM , as well as FoodEx2, are classification and description systems for indexing, in the sense of a systematic description, of foods based on a hierarchical model (parent-child relationship), thus facilitating the international exchange of data on food composition, consumption, assessing chronic and/or acute exposure to a certain agent, and not least the assessment of nutrient intake. The database, here presented, consists of the codes of fifty ready-to-eat products present on the market in Italy, obtained by using the two mostly commonly used and widely recognized coding systems: LanguaL TM and FoodEx2. This database represents a tool and a guideline for other compilers and users to apply coding systems to ready-to-eat products. Moreover, it can be represented a resource for several applications, such as nutritional cards, nutritional facts, food labels, or booklet and brochures for promotion of food products, to be used at health and food nutrition interface, useful for consumers, dieticians, and food producers.

The aim of this research was to develop innovative cheeses fortified with vitamin D3 (VD3). Formulation studies and analyses of textural properties and chemicals were carried out for these developments. Two traditional Italian varieties of cheese (giuncata and burrata) were studied. For giuncata, the fortification of milk for cheese production provided a VD 3 retention level of 43.9 ± 0.6% in the food matrix. For burrata, the VD 3 ingredient was incorporated into the creamy inner part after mixing, maintaining the textural quality of the product (adhesiveness 4.3 ± 0.4 J × 10 -3 ; firmness 0.7 ± 0.0 N; and cohesiveness 0.8 ± 0.2). The optimized enrichment designs allowed to obtain homogenous contents of VD 3 during the production of giuncata (0.48 ± 0.01 µg/g) and burrata cheeses (0.32 ± 0.02 µg/g). Moreover, analyses revealed the high stability of VD 3 during the storage of the two fortified cheese types (2 weeks, 4 °C). These fortification designs could be implemented at an industrial scale to obtain new cheese types enriched in VD 3 and thus contribute to the reduction in VD deficiency prevalence.

Even though microplastic (MP) pollution in aquatic environment is nowadays widely studied, a huge gap of knowledge exists on their actual biological effects. In this study we first reported environmental baseline data on the occurrence and characterization of floating MPs in Italian coastal waters of the Central Adriatic Sea by using a standardized monitoring protocol. Further, we analyzed the concentrations of MP-associated chemicals and evaluated their potential adipogenic effects using 3T3-L1 preadipocytes. MPs were found in each sampling stations showing the highest abundance (1.88 ± 1.78 items/m 3 ) in the sites more distant from the coast with fragments as the most common shape category. All targeted organic pollutants (i.e. polychlorinated biphenyls - PCBs, polycyclic aromatic hydrocarbons -PAHs, organophosphorus - OP, and organochlorine - OC pesticides) have been detected on the surface of the collected MPs. The highest concentrations of PAHs were found on MPs from inshore (i.e. <1.5 NM) surface waters with low-ring PAHs as dominant components. Similarly, MPs from inshore waters had higher ΣPCB concentrations (64.72 ng/g plastic) than those found in offshore (i.e. >6 NM) waters (10.37 ng/g plastic). Among pesticides, all measured OPs were detected in each sample analyzed with pirimiphos-methyl as the most representative compound. For OCs, the sum of all concentrations of congeners was higher in coastal with respect to offshore waters. Moreover, in vitro 3T3-L1 screening of MP extracts indicated potential metabolic effects resulting in both adipogenesis and lipid uptake/storage., 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. On behalf of all authors, the corresponding author states that there is no conflict of interest., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

This study was carried out to characterize extracts from nine samples of the apple 'Mela Rosa dei Monti Sibillini' (MR) and to assess the antioxidant and anti-inflammatory activities. The extracts were analysed by High Performance Liquid Chromatography coupled with photodiode array detector and mass spectrometry (HPLC-DAD-MS) for 20 phytochemicals. The extracts from the lyophilized material (ELM) were richer in polyphenolic compounds than the dried ones (EDM). The MR extracts contained noteworthy amounts of the investigated analytes compared to one sample of the commercial varieties Annurca, Golden Delicious and Granny Smith used as reference. Principal component analysis (PCA) revealed that the part of the fruit seems to have a significant influence on the chemical composition of the final extract; thus, the peel extracts exhibited higher levels of phenolic compounds, especially epicatechin, procyanidin B2 and phloridzin, and triterpenes than the pulp ones. In general, the lyophilized material showed higher antioxidant activity than the dried material. The strong antioxidant capacity of the MR has also been revealed by the DPPH, ABTS, FRAP and Folin-Ciocalteau assays. The ELM of MR significantly reduced reactive oxygen species in lipopolysaccharide (LPS)-activated mouse brain microglia cells (BV-2 cells). Real-time polymerase chain reaction (RT-PCR) analysis demonstrated that the EDM and ELM of MR were effective in reducing pro-inflammatory cytokines and enzymes in BV-2 and peripheral blood mononuclear cells (PBMC). These results contribute to the exploitation of this ancient variety as a source of nutraceuticals., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

2-Isopropylmalic acid (2-IPMA) and 3-isopropylmalic acid (3-IPMA), recently discovered in wines, were simultaneously quantified in forty wines by UHPLC-MS/MS triple quadrupole. Principal component analysis displayed that red wines were more correlated with high amounts of 2-IPMA (average content 31.60 mg/L); white wines were mostly characterized by low levels of both organic acids. No correlation of theirs levels to other wine features (wine ageing or alcoholic content) were found. 2-IPMA and 3-IPMA showed MICs values of 4096 mg/L and MBCs values of 8192 mg/L or higher against several food borne pathogens. In association, an interesting lower MIC and MBC values (2048 mg/L and 4096 mg/L respectively) were observed against Y. enterocolitica. Interestingly, 3-IPMA showed a mild antioxidant activity by DPPH assay (EC 50  = 3940 mg/L), higher than that of 2-IPMA (EC 50  > 4800 mg/L). No toxicity of these compounds against human colorectal and liver cells (TB assay) was observed., 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 © 2020 Elsevier Ltd. All rights reserved.)

The effect of feeding supplementation on the nutritional characteristics of milk and cheese was studied in dairy sheep grazing on low mountain dry-grasslands during summer in typical sub-Mediterranean conditions of aridity. The control group (CG) of 25 sheep grazed on grass, while the experimental group (EG) of 25 sheep grazed on grass and received 600 g a day of a barley and corn mixture. Daily milk production showed a less pronounced decrease in EG than in CG ( p ˂ 0.0368). After one month of supplementation, the concentrations of retinol and α-tocopherol in milk and cheese from EG were higher than CG ( p  < 0.05). Supplementary feeding had a positive effect on the fatty acid composition of the sheep milk. For the first time, positive effects on the volatile composition were found in EG cheese, displaying lower percentages of carboxylic acids associated with the pungent and rancid odour with respect to CG.

Organic acids of wine comprise one of the main taste groups, that of sourness. Two isomeric compounds with molecular weight of 176 u have been identified in wine using two LC-MS systems, LC-IT (ion trap) and LC-Q-Orbitrap. The two isomers are organic acids, 3-isopropylmalic acid (3-IPMA) never identified in wines, and 2-isopropylmalic acid (2-IPMA), never quantified in wines. After the definitive identification against the authentic standards, an analytical method for their determination in wines was optimised and validated using the LC-IT platform. Linearity was verified in the range 5-320 mg L -1 (correlation coefficients higher than 0.9914) and the recoveries obtained spiking the samples at two fortification levels were higher than 86.7%, with RSDs (n = 9) lower than 15.1%. Finally, the two compounds were quantified in ten red and white Italian wines, and average concentrations were determined at 1.78 mg L -1 (0.56-4.13) and 23.0 mg L -1 (6.7-41.6) of 3-IPMA and 2-IPMA, respectively., (Copyright © 2019 Elsevier Ltd. 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.)

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.

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.)

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.)

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.)

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.)

The chemical composition of the essential oils of nine taxa from seven sections of Hypericum L. (Guttiferae; H. perforatum subsp. perforatum, H. perforatum subsp. veronense, H. calycinum, H. montanum, H. richeri subsp. richeri, H. hyssopifolium, H. hirsutum, H. hircinum subsp. majus, and H. tetrapterum) occurring in central Italy (Appennino Umbro-Marchigiano) was analyzed by GC/FID and GC/MS. A total of 186 compounds were identified in the different species and subspecies, accounting for 86.9-92.8% of the total oils. The major fraction of the oil was always represented by sesquiterpene hydrocarbons (30.3-77.2%), while quantitative differences occurred between the other classes of volatiles depending on the taxa considered. Chemical composition of the nine Hypericum entities with respect to the taxonomical classification was discussed. Essential oils obtained from six taxa, i.e., H. perforatum subsp. perforatum, H. perforatum subsp. veronense, H. calycinum, H. richeri subsp. richeri, H. hirsutum and H. tetrapterum, were also tested for their antimicrobial properties against five different microbial strains by the broth-microdilution method, and they were found to have significant activity (expressed as MIC) on B. subtilis, moderate activity on C. albicans and S. aureus, and weak activity on E. coli and E. faecalis, the most active being those from H. hirsutum, H. richeri subsp. richeri, and H. tetrapterum.

Lentil saponins are triterpene glycosides, mainly soyasaponins I and betag (also known as VIota), with multiple health-promoting properties. This paper reports the isolation of soyasaponins I and betag from soybeans as analytical standards and the development of a new analytical procedure for quantification of their content in various cultivars of Italian lentils, by SPE-HPLC-MS. Soyasaponins I and betag were isolated from soybeans at a purity of >90% and characterized by MS/MS (ion trap) experiments. The determination of soyasaponins in lentils was performed by extraction, SPE purification, and HPLC-MS (single quadrupole) analysis; results were confirmed by MALDI-TOF experiments. Calibration curves for soyasaponin I and betag showed correlation coefficients of 0.998 and 0.997, respectively. LOD and LOQ values were 0.02 and 0.2 mg kg(-1) for soyasaponins I and 0.1 and 1 mg kg(-1) for soyasaponin betag. Recoveries calculated at a 100 mg kg(-1) fortification level ranged from 85 to 97%, with n = 10 and RSDs of <12%. In the 32 lentil samples, contents of soyasaponin I ranged from 28 to 407 mg kg(-1), whereas that of soyasaponin betag ranged from 110 to 1242 mg kg(-1).

The essential oil obtained from different parts of Ferula glauca L. (formerly considered as a subspecies of F. communis) growing in Marche (central Italy), was analyzed for the first time by GC-FID and GC-MS. The major volatiles were (E)-caryophyllene and caryophyllene oxide in leaves, alpha-pinene, myrcene and germacrene D in flowers, alpha- and beta-pinene in fruits, (E)-beta-farnesene, myristicin and elemicin in roots, respectively. The differences in composition detected with respect to F. communis, made the volatile fraction a reliable marker to distinguish between them, and confirm the botanical data at the base of their discrimination. Furthermore, the oil was assayed for its antimicrobial activity by the broth microdilution method. B. subtilis was found to be the most sensitive microorganism, with the lowest MIC values.

Levels of 18 polychlorinated biphenyl (PCB) congeners were determined by gas chromatography-mass spectrometry (GC-MS) in some marine species, living both in the coastal area and in deeper seawater. In some species analysis was performed separately in edible parts (fillets) and in viscera. The existence and degree of bioaccumulation was assessed studying individual species of very different size, with the smaller being younger. Furthermore, with a multivariate statistical analysis, a correlation between PCB congeners and the feeding habits and habitat of the fish was demonstrated. The results show that fat from edible parts (fish fillets) had total PCB levels in the range 22.6-601.9 µg kg⁻¹ (with 601.9 µg kg⁻¹ in anchovies), while fat from viscera showed much higher concentrations (407.3-916.6 µg kg⁻¹). Bioaccumulation was confirmed, comparing PCB levels between younger and older individual hake, squid, and horned octopus. The total PCB concentration ratio (older/younger individuals) ranges from 2.11 (squid = 292.1/137.8 µg kg⁻¹) to 3.46 (hake = 546.0/158.0 µg kg⁻¹).

Methanol-acetone extracts from aerial parts of seven entities of the genus Hypericum [H. perforatum L. subsp. perforatum, H. perforatum L. subsp. veronense (Schrank) Ces., H. montanum L., H. hyssopifolium Chaix, H. hirsutum L., H. hircinum L. subsp. majus (Aiton) N. Robson, H. tetrapterum Fr.] growing in the Appennino Umbro-Marchigiano (central Italy) were tested in vitro for their antimicrobial activity against two Gram-positive bacteria (Staphylococcus aureus and Enterococcus faecalis), two Gram-negative bacteria (Escherichia coli and Pseudomonas aeruginosa) and the yeast Candida albicans, by the Kirby-Bauer agar diffusion method. The two H. perforatum subspecies were particularly active against Gram-positive and Gram-negative bacteria, supporting the use of these plants in the traditional medicine of central Italy to treat wounds, skin and infectious diseases. However significant values of inhibition were given also by H. hirsutum against S. aureus and P. aeruginosa, and by H. hyssopifolium, H. hircinum subsp. majus and H. tetrapterum against C. albicans. These results suggest that hypericin and hyperforin are the main components responsible for antimicrobial activity, but not the only ones, as other extracts, showing a low level of these compounds, possess evident activity. Isolation of pure compounds from the most active extracts is in progress.