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A greenhouse pot experiment was conducted to evaluate the impact of zinc supply (0, 1, and 2 mM Zn as ZnSO

In this work, four triazole-based poly(ether-pyridine)s polymers were synthesized and used as an adsorbent for the removal of phenolic compounds from aqueous solutions. For this purpose, new fluoromonomers containing 1,2,3-triazole units were prepared by the Cu(I)-catalyzed 1,3-dipolar cycloaddition reaction and then used for the elaboration of novel poly(ether-pyridine-triazole)s (PEPTs) by direct polycondensation with isosorbide and bisphenol A. Chemical structure of fluorinated pyridinic monomers as well as resulting polymers was confirmed by 1 H and 19F NMR spectroscopic methods. The thermal behavior of the obtained PEPTs was characterized using differential scanning calorimetry and thermogravimetric analysis. Results of sorption showed that polymers can be effectively used as a sorbent for the removal of polar organic pollutants. The isosorbide-based poly(ether-pyridine-triazole) which contains hydrophilic hydroxyl groups as pendants chains (P4) exhibited the highest sorption efficiencies (78%–100% after 1 h). In order to explain the results an adsorption mechanism mainly based on π–π interactions and hydrogen bonding with the pendent groups is proposed. &nbsp

The present study aims to investigate the effect of copper (as CuSO4, 5H2O) supply (0, 25 and 50 μM) on performance of cilantro (Coriandrum sativum L.) plants grown under hydroponic conditions. All applied Cu concentrations drastically reduced the biomass production, length of the shoots and the roots and disturbed the ions (Cu, Ca, Fe, Zn and Mg) homeostasis. Either Cu-starvation (0 μM) or Cu-toxicity (25 and 50 μM) significantly reduced the net photosynthetic rate, stomatal conductance and transpiration rate resulting in reduced water use efficiency. Under Cu-toxicity, the variations in gas exchange parameters were associated with a remarkable decline in the photosynthetic pigments including Chlorophyll a, Chlorophyllb, Chlorophyll (a + b) and carotenoids. Additionally, an enhanced lipid peroxidation (evaluated as Malondialdehyde (MDA) contents) with a concomitant increase in proline, total soluble sugars and melanoidins contents were observed under these conditions. The increased MDA levels resulted in decrease in total lipid content and alteration of the fatty acid profiles in both shoots and roots with a general tendency toward the accumulation of saturated fatty acids that mirrors a decline in the desaturases activity. Although the increased activity of enzymatic antioxidants including catalase (CAT), gaiacol peroxidase (GPX) and ascorbate peroxidase (APX), the oxidative-induced injuries caused by 25 and 50 μM Cu were found to be irreversible and the optimal growth parameters were not achieved.

For the development of selective and sensitive chemical sensors, we have developed a new family of poly(etherphosphoramide) polymers. These polymers were obtained with satisfactory yields by nucleophilic aromatic polycondensation using isosorbide as green resources, and bisphenol A with two novel difluoro phosphinothioic amide monomers. Unprecedented, the thiophosphorylated aminoheterocycles monomers, functionalized with two heterocyclic amine, N-methylpiperazine and morpholine were successfully obtained by nucleophilic substitution reaction of P(S)–Cl compound. The resulting polymers were characterized by different analytical techniques (NMR, MALDI–ToF MS, GPC, DSC, and ATG). The resulting partially green polymers, having tertiary phosphine sulfide with P–N side chain functionalities along the main chain of polymers are the sensitive film at the surface of a gold electrode for the impedimetric detection of Cd, Ni, Pb and Hg. The bio-based poly(etherphosphoramide) functionalized with N-methylpiperazine modified sensor showed better analytical performance than petrochemical based polymers for the detection of Ni2+. A detection limit of 50 pM was obtained which is very low compared to the previously published electrochemical sensors for nickel detection

Natural plant extracts are primarily used as raw materials in the cosmetic and perfumery industry. However, adulterations with petrochemical products are occurring in the market, leading to non-100% natural products. Several analytical techniques such as impurity detection or enantioselective ratio assessments have been previously described as good indicators to detect any addition of synthetic products, but these techniques are ineffective with novel type of synthetic pathways such as semisynthesis. In order to improve authentication, development of advanced analytical strategies such as δ

Citation suggérée:Anses (2021). Priorisation des substances chimiques à rechercher dans les émissions des produits du vapotage en vue de l’évaluation des risques sanitaires. Rapport d’expertise collective (saisine 2020-SA-0016). Maisons-Alfort : Anses, 57 p.; La directive 2014/40/UE sur les produits du tabac établit des règles concernant la fabrication, la présentation et la vente des produits du tabac et produits connexes. Elle instaure notamment une obligation de déclaration1 des produits avant toute commercialisation. Cet enregistrement des produits ne relève pas d’un processus d’autorisation de mise sur le marché.Les produits du tabac et produits connexes sont classés en trois catégories :- Les produits du tabac ;- Les produits du vapotage ;- Les produits à fumer à base de plantes autres que le tabac.Certaines informations à transmettre sont communes à ces trois catégories de produits notamment la composition en ingrédients et additifs avec leurs quantités. D’autres informations sont spécifiques à la catégorie : il s’agit notamment des mesures à l’émission de composés formés lors de l’utilisation des produits du vapotage.La déclaration auprès des autorités de chaque État membre concerné est un processus informatique centralisé selon les modalités du point d'entrée électronique commun de l'Union européenne. Mis au point par la Commission européenne, il est opérationnel pour réceptionner les déclarations depuis le 20 mai 2016, date d’entrée en application de la directive.En France, la directive 2014/40/UE a été transposée par l’ordonnance N°2016-623 du 19 mai 2016 qui introduit les nouvelles dispositions au titre Ier du livre V de la troisième partie du Code de la santé publique (CSP). Les décrets des 11 et 22 août 2016 ainsi que les arrêtés du 19 mai et 22 août 2016 complètent les dispositions règlementaires nationales. L’autorité administrative compétente est le ministère chargé de la santé.Dans le cadre de cette transposition, l’Agence nationale de sécurité sanitaire de l’alimentation, de l’environnement et du travail (Anses) a été désignée pour assurer la réception, le stockage, le traitement et l’analyse des informations transmises par les déclarants sur leurs produits.L’obligation règlementaire de déclarer ces informations doit permettre d’améliorer les connaissances quant à la composition des produits, l’impact sur la santé et l’évolution de la demande et de l’offre des produits du tabac et produits connexes.En outre, certains ingrédients et additifs sont interdits : il s’agit notamment des substances cancérogènes, mutagènes et toxiques pour la reproduction, des vitamines, des stimulants tels que la caféine ou la taurine (articles L. 3512-16 et L. 3513-7 CSP).Mi-2020, plus de 33 000 produits du vapotage ont été enregistrées sur le marché français. La mission confiée à l’Anses se traduit par la conduite de travaux d’expertise portant sur l’identification et l’évaluation des dangers des substances chimiques auxquelles le consommateur ou son entourage sont exposés lors de l’utilisation de ces produits. Au-delà de la fumée de tabac dont les effets sanitaires sont connus, l’enjeu porte plus particulièrement sur les substances émises par les produits du vapotage et les nouveaux produits du tabac chauffé lors de leur utilisation.[Saisine liée « 2018-SA-0189 , Produits du tabac : bilan 2016 - 2020 »]

Pure and natural essential oils of Allium species are primarily used in the food industry, but due to their low yield, production quantities can be difficult to achieve and thus can be highly expensive. Due to these problems, adulterations are a reality in this field. The purpose of this research is to develop a multi element stable isotope analysis methodology for authentication of the essential oils of leek, onion, shallot, and chive. Naturalness of these essential oils was achieved by assessment of compound specific δ13C and δ34S: an addition of 5% of synthetic compound can be detected. Chemometric models were undertaken to assess purity by distinction of the Allium samples according to their species origin using bulk stable and compound specific δ13C, δ2H, δ34S, and compositions of their major metabolites dipropyl disulfide, dipropyl trisulfide, methyl propyl disulfide, and methyl propyl trisulfide.

The effects of cement dust on the yield and chemical composition of the essential oil were investigated in Cupressus sempervirens. Exposure to cement dust resulted in a significant increase in the essential oil yields. Significant factory distance-related changes in qualitative and quantitative composition of the essential oil were observed. Increasing pollution with dust increased the content of monoterpene hydrocarbons concomitant to increase of α-pinene, suggesting a redirection of the secondary metabolism of C. sempervirens towards biosynthesis of monoterpenes. In contrast, oxygenated monoterpenes and sesquiterpene hydrocarbons were strongly reduced. These results provide an overall picture of the different responses of monoterpenes and sesquiterpenes to air pollution caused by cement dust. They also reveal the suitability of using C. sempervirens in the creation of green areas around cement factories and encourage the use of dusted plants as potential source of valuable natural products. Keywords: Cement dust, Cupressus sempervirens, Essential oil, Monoterpenes, Environmental pollution

Phenolic and substituted phenol based resoles are commonly used in the formulation of can coatings. However, migration analyses of these coatings are very little described compared to other coating technologies. While epoxy and polyester have well known migrants with defined formation mechanisms, Non-Intentionally Added Substances (NIAS) specifically related to the phenolic resin are hardly studied in the literature. The goal of the publication is to further explore the influence of the phenolic resole, used in the formulation of can coatings, on extracted NIAS's nature. Six different model polyester-phenolic can coatings were formulated each with a specific phenol, cresol or tertbutylphenol-based resole. Can coating films were extracted for 24 h at 40 °C in acetonitrile before analysis. NIAS identification was done using gas chromatography separation coupled to high resolution mass spectrometry (HRMS) and nuclear magnetic resonance (NMR) spectroscopy analyses. Cyclic polyester oligomers were found in all extracts, with oligomers found in a range of 10 μg/dm

In this work, innovative biosourced polyimide polymers were derived from novel combinations of monomers (Isosorbide, 6-FDA and amine cardo). These polymers were obtained with satisfactory yields by polycondensation of different percentages of isosorbide and of 6-FDA (from 100% to 0%). The synthesized polyimides had number average molecular weight in the 17,600–22,000 g/mol range, and they were stable well above 451 °C (5% weight loss in N2). The glass transition temperature (Tg) were found to be in the range of 318–414 °C, depending on the composition of the copolymers. The adsorption of Water Framework Directive (WFD) heavy metals (Pb2+, Ni2+, Cd2+, Hg2+) on the biosourced polyimide films deposited on a gold electrode was monitored by the measurements of the impedance of the electrolyte/polyimide polymer/electrode interface. The adsorption isotherm of Pb2+on the different polyimide films was modeled according to a Langmuir isotherm with a best fitting. The relative adsorption capacities were higher when the isosorbide content was higher. Comparing the adsorption capacities of the different WFD heavy metals of the isosorbide based polyimide, the sequence is the following one: Pb2+ ≈ Ni2+ > Cd2+ > Hg2+. These results are within the paradigm of Pearson’s HSAB principle about the metal-oxygen interaction. When isosorbide based polyimide is the sensitive part of an impedimetric sensor, the detection limit for all the WFD heavy metals is 50 pM, very lower than the environmental quality standards for these WFD priority hazardous substances.

In this work, impedimetric sensors were developed for the detection of the four WFD heavy metals Pb2+, Cd2+, Hg2+ and Ni2+, by the modification of a gold electrode with four partially biosourced polyphosphine polymers. These polymers were obtained with satisfactory yields by polycondensation of the bis(4-fluorophenyl)(4-methylphenyl)phosphine sulfide and the bis(4-fluorophenyl)(4-methylphenyl)phosphine oxide using isosorbide or bisphenol A. The chemical structures and number-average molecular weights of the resulting polymers were determined by NMR spectroscopy (1H, 19F, and 31P) and by size exclusion chromatography. Glass transition temperatures varied between 184 and 202 &deg, C depending on the composition of polymers. The bio-based poly(etherphosphine) oxide modified sensor showed better analytical performance than petrochemical based oxide for the detection of Pb2+. A detection limit of 10&minus, 10 g/L or 0.5 pM, which is 104 times lower than that of the anodic stripping voltammetric and the potentiometric sensors. A reversibility is obtained through rinsing of the impedimetric sensor with an EDTA solution.

National audience

The essential oil of wintergreen, which is extracted by steam distillation from Gaultheria genus leaves, is mainly used in aromatherapy. However, due to its adulteration easiness with synthetic material, it is necessary to control samples naturalness with accuracy. The purpose of this work was to develop a methodology to authenticate the essential oil of wintergreen. Wintergreen essential oil is composed of more than 99% methyl salicylate. This aromatic ester can be easily synthesized and used to adulterate wintergreen essential oil. Authentic wintergreen essential oil can be distinguished from adulterated oils by examining their compositions. The detection of methyl salicylate synthetic marker compounds (methyl 4-hydroxybenzoate, dimethyl 4-hydroxyisophthalate or dimethyl 2-hydroxyisophthalate) or the absence of several naturally occurring minor secondary metabolites (ethyl salicylate and vitispirane) contribute to the authentication. Isotopic values of bulk wintergreen essential oil have also been determined using an isotope ratio mass spectrometer (IRMS): the δ13C values of authentic samples range from −36.78 to −33.36‰, the δ2H values range from −173 to −115‰ and the δ18O values range from −1.3 to 5.7‰. However, these analytical methods cannot account for the natural variability in the essential oils. To determine the boundaries of the natural isotopic values, 14C radioactive isotope activity assessment was undertaken, which allows for the determination of the genuineness of samples that are not assessed using multistable isotope approaches. Additional studies evaluating 14C activity of a noncompliant sample using IRMS identified a 14C-labeled synthetic methyl salicylate adulteration.

Neroli essential oil (EO), extracted from bitter orange blossoms, is one of the most expensive natural products on the market due to its poor yield and its use in fragrance compositions, such as cologne. Multiple adulterations of neroli EO are found on the market, and several authentication strategies, such as enantioselective gas chromatography (GC) and isotope ratio mass spectrometry (IRMS), have been developed in the last few years. However, neroli EO adulteration is becoming increasingly sophisticated, and analytical improvements are needed to increase precision. Enantiomeric and compound-specific isotopic profiling of numerous metabolites using multidimensional GC and GC-C/P-IRMS was carried out. These analyses proved to be efficient for geographical tracing, especially to distinguish neroli EO of Egyptian origin. In addition, δ2H values and enantioselective ratios can identify an addition of 10% of petitgrain EO. These results demonstrate that enantioselective and stable isotopic metabolite fingerprint determination is currently a necessity to control EOs.

Royal jelly, a honey bee secretion, plays a critical role in caste determination in honey bees because it serves as the source of nutrition for young larvae destined to become queens. It is also fe...

Changes in fatty acid profile, lipid quality, essential oil composition, total phenolic (TPC) and flavonoid (TFC) contents, radical scavenging, antibacterial and insecticidal activities were studied during the maturation of Schinus terebinthifolius Raddi fruits. Total lipids showed their maximum at the earlier and intermediate stage (green and half-red) of maturation, whereas, the highest levels of the main components linoleic and oleic acids were found at the late stage (red). Mature fruits were also distinguished by their high lipid quality as revealed by the lower values of n-3/n-6 ratio, calculated oxidizability (Cox), oxidative susceptibility (OS), atherogenic index (AI) and thromobogenic index (TI). The contents of monoterpenes decreased while those of sesquiterpenes increased during maturation. With the exception of α-pinene which dropped remarkably from immature to mature fruits, the content of the other main components (α-phellandrene, β-phellandrene and limonene) showed irregular variations. The TPC in intact and hydrodistilled fruits was higher at the last stage of maturation, while the maximum of TFC was recorded in the intermediate stage. Concomitantly, extract from residual hydrodistilled fruits was found as the most potent radical scavengers, whereas, the oils were found as the least scavengers. Nevertheless, they showed an appreciable antibacterial activity against Enterococcus feacium and Streptococcus agalactiae and exert a strong insecticidal activity against Spodoptera littoralis and Phthorimaea operculella . Collectively, these results suggest that the fruits of S. terebinthifolius could be considered as consolidated source of lipid and essential fatty acids, which may provide some health benefits to consumers. They also showed that the essential oils of S. terebinthifolius fruits can potentially be used in S. littoralis and P. operculella control in association with integrated pest management practices. Moreover, the use of extracts from intact or hydrodistilled residual fruits for the development of functional ingredients and the production of bio-based preservatives is encouraged.

In this study, peroxidases (PODs) from three waste by-products: broad bean pods (BBP), pea pods (PP), and artichoke stems (ARS) were purified and their optimal conditions were determined for the first time. The purification process resulted in 4.32, 7.21, and 8.9% of POD recoveries for PP, ARS, and BBP, respectively. They were purified 2.12-, 32.97-, and 10-fold with specific activities of 27.26, 266.43, and 27 U/mg of protein, respectively. Analysis of their optimal conditions showed that POD purified from BBP and PP exhibited the highest activity at 60 °C temperature and pH 6 and 8 with strong affinity with catechol substrate (Km of 0.356 and 0.189 mM; Vmax of 0.08 and 0.041 μM/min for BBP and PP, respectively). The highest activity of ARS POD was obtained under the following conditions: temperature at 50 °C, pH from 6 to 8, and guaiacol as substrate (Km 0.375 mM; Vmax 0.012 μM/min). Apart from giving the opportunity for recycling the food industry wastes, the studied waste by-products could represent an alternative source of PODs that could find several applications in the biotechnological, chemical, and food industries.

Four Semi-Interpenetrating Networks (semi-IPN) based on polydimethylsiloxane (PDMS) were developed for the sorptive extraction of polar phenolic compounds (log Kow ≤ 3). Their preparation is based on the hydrosilylation crosslinking reaction of dihydrosilane terminated polydimethylsiloxane with its homologue divinyl, followed by the addition of inert various polyethylene oxide derivatives (PEO). The physico-chemical properties of the semi-IPN were controlled by Differential Scanning Calorimetry (DSC), Scanning Electronic Microscopy (SEM), RAMAN spectroscopy and contact angle measurements, showing the homogeneity of the semi-IPN and their higher hydrophilicity. Under optimum extraction conditions of phenolic molecules as target analytes and using liquid chromatography as analysis techniques, the novel modified PDMS phases showed good extraction rate against polar analytes with an excellent relative recovery average (69–100 %) for phenolic molecules. The higher retention rates were obtained with 30 % interpenetrated copolymer PEO/PPO in PDMS. Moreover, five adsorption/desorption cycles led to a loss of 5.8 % of the adsorption efficiency, showing a good stability of these PDMS-based IPN phases.

International audience; Plant-based remedies have been widely used for the management of variable diseases due to their safety and less side effects. In the present study, we investigated Saussurea lappa CB. Clarke. (SL) given its largely reported medicinal effects. Specifically, our objective was to provide an insight into a new polymethyl methacrylate based nanocapsules as carriers of SL essential oil and characterize their biologic functions. The nanoparticles were prepared by nanoprecipitation technique, characterized and analyzed for their cytotoxicity, anti-inflammatory, anti-Alzheimer and antidiabetic effects. The results revealed that the developed nanoparticles had a diameter around 145 nm, a polydispersity index of 0.18 and a zeta potential equal to +45 mV and they did not show any cytotoxicity at 25 μg·mL−1. The results also showed an anti-inflammatory activity (reduction in metalloprotease MMP-9 enzyme activity and RNA expression of inflammatory cytokines: TNF-α, GM-CSF and IL1β), a high anti-Alzheimer’s effect (IC50 around 25.0 and 14.9 μg·mL−1 against acetylcholinesterase and butyrylcholinesterase, respectively), and a strong antidiabetic effect (IC50 were equal to 22.9 and 75.8 μg·mL−1 against α-amylase and α-glucosidase, respectively). Further studies are required including the in vivo studies (e.g., preclinical), the pharmacokinetic properties, the bioavailability and the underlying associated metabolic pathways.

International audience; In the present work, we propose the synthesis of a new family of sugar derived 1,4:3,6-dianhydrohexitol based AA/AB-type monomers. Unprecedented diacids based on Isomannide and Isoidide were elaborated with high yields and showed interestingly high melting point ranges (240-375 degrees C). Optimization of reaction conditions (temperature, time of reaction, and reactant ratios) has been investigated to synthesize the key intermediate of a set of AB monomers with acid, ester, and acid chloride functionalities. Isosorbide based ether benzoic acid AB monomer was polymerized and characterized by NMR and DSC techniques. The results show a semicrystalline behavior of the obtained polymer thanks to the controlled stereoregular arrangement of the AB starting monomer.

In a stricter legislative context, greener detergent formulations are developed. In this way, synthetic surfactants are frequently replaced by bio-sourced surfactants and/or used at lower concentrations in combination with enzymes. In this paper, a LC-MS/MS method was developed for the identification and quantification of enzymes in laundry detergents. Prior to the LC-MS/MS analyses, a specific sample preparation protocol was developed due to matrix complexity (high surfactant percentages). Then for each enzyme family mainly used in detergent formulations (protease, amylase, cellulase, and lipase), specific peptides were identified on a high resolution platform. A LC-MS/MS method was then developed in selected reaction monitoring (SRM) MS mode for the light and corresponding heavy peptides. The method was linear on the peptide concentration ranges 25-1000 ng/mL for protease, lipase, and cellulase; 50-1000 ng/mL for amylase; and 5-1000 ng/mL for cellulase in both water and laundry detergent matrices. The application of the developed analytical strategy to real commercial laundry detergents enabled enzyme identification and absolute quantification. For the first time, identification and absolute quantification of enzymes in laundry detergent was realized by LC-MS/MS in a single run. Graphical Abstract Identification and quantification of enzymes by LC-MS/MS.

RATIONALE To develop more eco-friendly laundry detergents, renewable surfactants synthesized from vegetal sources are increasingly being used. In a more stringent regulation context, the determination of bio-sourced surfactant origin thus appears essential to assess the claims of detergent manufacturers. Radiocarbon determination, the standard method for the analysis of bio-sourced materials, is an expensive technique, so there is a need for a cheaper method. METHODS Here, the use of an elemental analyzer linked to isotope-ratio mass spectrometry (EA/IRMS) is evaluated as an alternative approach to the official method. The δ(18) O, δ(13) C and δ(2) H isotope-ratio values were determined to investigate the bio-sourced origin of surfactant raw materials and mixtures. RESULTS A sample library of 26 commercial surfactants representative of detergent raw materials was first analyzed by EA/IRMS. The δ(18) O, δ(13) C and δ(2) H values allowed discrimination of synthetic and bio-sourced surfactants. Moreover, in this latter group, C4 plant-derived surfactants were distinguished by their δ(13) C values. Binary and ternary mixtures made of synthetic and bio-sourced surfactants were also analyzed and indicated a linear relationship between mixture isotope-ratio values and surfactant proportions. CONCLUSIONS IRMS represents a viable alternative to radiocarbon determination for the evaluation of surfactant bio-sourced origin. It is a faster and cheaper technique, allowing discrimination of petroleum- and biomass-derived surfactants and identification of their carbon sources (C4 or C3 plants).

The composition of the fatty acids of the roots and aerial parts of Aritolochia longa (Aristolacheae) and Bryonia dioica (Cucurbutaceae) was analyzed by gas chromatography (GC-FID) and gas chromatography-mass spectrometry (GC-MS). The oils extracted from the aerial parts of both species were rich in polyunsaturated fatty acids with the essential linolenic and linoleic acids being the most prominent compounds. Oleic and linoleic acids were the majors fatty acids in the roots of both species. Whatever the plant part analyzed and the species, the saturated fatty acids were predominantly composed of palmitic and stearic acids. The antibacterial activity, minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of the lipid extracts were determined against a panel of five bacterial strains. The results showed that the sensitivity to the lipid extracts was different for the test bacterial strains, and the susceptibility of gram positive bacteria was found to be greater than gram negative bacteria. The antibacterial activity of the root lipid extracts was particularly important against Enterococcus feacium (CMI value of 125 µg/mL; CMB values > 250 µg/mL) and Streptococcus agalactiae (CMI value of 125 µg/mL; CMB values 250 µg/mL for A. longa roots). These results indicate that A. longa and B. dioica could be considered as good sources of essential fatty acids which can act as natural antibacterial agents.

Enzyme-assisted extraction has emerged as an attractive green, cost-effective and high bioactive yielding technology by which desired bioactives with preserved or better efficacy are released. In the present study, the ability of cellulase, hemicellulase and their binary mixture (cellulase:hemicellulase; 1:1) in improving the extraction of essential oils from coriander (Coriandrum sativum L.) seeds, or the residue by-products from the distillation process containing value-added phytochemicals (fatty acids and phenolics) were evaluated. Cellulase and the binary mixture improved the extraction of essential oils by 44.2 and 40%, respectively. Application of enzymes was associated with increased amount of oxygenated terpenes in the essential oils derived from enzyme-treated samples. Linalool, camphor and geranyl acetate were the prominent compounds. From the hydrodistillation residues, a better recovery of petroselinic-rich oil with a good nutritional quality was also observed in enzyme-treated seeds. They also contained an appreciable amount of polyphenols and showed an improved antioxidant activity as revealed by the DPPH, FRAP and cellular antioxidant activity assays. The results suggested that enzyme pre-treatment allowed better recovery without alteration of the essential oil composition. The hydrodistillation residues obtained could be potentially exploited for the development of functional food ingredients and nutraceuticals.

Enzyme-assisted extraction has emerged as an attractive green, cost-effective and high bioactive yielding technology by which desired bioactives with preserved or better efficacy are released. In the present study, the ability of cellulase, hemicellulase and their binary mixture (cellulase:hemicellulase; 1:1) in improving the extraction of essential oils from coriander (Coriandrum sativum L.) seeds, or the residue by-products from the distillation process containing value-added phytochemicals (fatty acids and phenolics) were evaluated. Cellulase and the binary mixture improved the extraction of essential oils by 44.2 and 40%, respectively. Application of enzymes was associated with increased amount of oxygenated terpenes in the essential oils derived from enzyme-treated samples. Linalool, camphor and geranyl acetate were the prominent compounds. From the hydrodistillation residues, a better recovery of petroselinic-rich oil with a good nutritional quality was also observed in enzyme-treated seeds. They also contained an appreciable amount of polyphenols and showed an improved antioxidant activity as revealed by the DPPH, FRAP and cellular antioxidant activity assays. The results suggested that enzyme pre-treatment allowed better recovery without alteration of the essential oil composition. The hydrodistillation residues obtained could be potentially exploited for the development of functional food ingredients and nutraceuticals.

International audience; The fatty acid, essential oil compositions and their respective antioxidant and antibacterial activities was determined in Schinus terebinthifolius Raddi leaves and twigs. The lipid content ranged from 1.75 to 4.65% in twigs and leaves, respectively. Thirteen fatty acids were identified with α-linolenic (C18:3), palmitic (C16:0) and linoleic (C18:2) acids being the main components. The essential oils of both organs were characterized by a high amount of monoterpene hydrocarbons (68.91-74.88%) with α-phellandrene (33.06-36.18%), α-pinene (14.85-15.18%) and limonene (6.62-8.79%) being the chief components. The DPPH˙ radical scavenging assay revealed that both oils have a very weak antiradical activity. In contrast, they showed an appreciable antibacterial activity against the gram-positive Enterococcus feacium (ATCC 19434) and Streptococcus agalactiae (ATCC 13813) bacteria. These results suggest that leaves and twigs of S. terebinthifolius could be considered as an important dietary source of health promoting phytochemicals and has a good potential for use in food industry and pharmacy.

The fatty acid, essential oil compositions and their respective antioxidant and antibacterial activities was determined in Schinus terebinthifolius Raddi leaves and twigs. The lipid content ranged from 1.75 to 4.65% in twigs and leaves, respectively. Thirteen fatty acids were identified with α-linolenic (C18:3), palmitic (C16:0) and linoleic (C18:2) acids being the main components. The essential oils of both organs were characterized by a high amount of monoterpene hydrocarbons (68.91–74.88%) with α-phellandrene (33.06–36.18%), α-pinene (14.85–15.18%) and limonene (6.62–8.79%) being the chief components. The DPPH˙ radical scavenging assay revealed that both oils have a very weak antiradical activity. In contrast, they showed an appreciable antibacterial activity against the gram-positive Enterococcus feacium (ATCC 19434) and Streptococcus agalactiae (ATCC 13813) bacteria. These results suggest that leaves and twigs of S. terebinthifolius could be considered as an important dietary source of health promoting phytochemicals and has a good potential for use in food industry and pharmacy. ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (10.1007/s13197-018-3049-6) contains supplementary material, which is available to authorized users.

International audience; Bay leaves (Laurus nobilis L.) are widely used as a condiment and their therapeutic benefits are well known. These biological properties were attributed to a plethora of highly bioactive secondary metabolites namely essential oils and phenolics. However, their recovery from plant matrix is generally limited by the presence of physical barrier (cell wall). Thus, the use of novel extraction procedures to enhance their release is particularly important. Therefore, the aim of this work is to assess the potential use of enzyme treatment (cellulase, hemicellulase, xylanase end the ternary mixture of them) as a tool to improve the extraction efficiency of bioactive compounds from bay leaves. Results showed that enzyme pre-treatment resulted in 243, 227, 240.54 and 0.48% increase in the essential oil yields in samples treated with cellulase, hemicellulase, xylanase and the ternary mixture, respectively. Compositional analysis by GC and GC MS revealed remarkable enrichment of the essential oils derived from enzyme-treated samples with oxygenated monoterpenes, leading hence to better antioxidant activity as revealed by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) and azino-bis-(3-ethylbenzothiolzoline 6-sulphonic acid) (ABTS) assays. The 1,8-cineole, alpha-terpinyl acetate, methyl eugenol, linalool, a-pinene, sabinene and beta-pinene were found as the most prominent components in all essential oils. Most importantly, enzyme treatment did not induce transformation of the volatile components, but it contributes to the liberation of some glycosidically bound volatiles. Moreover, it significantly enhances the release of phenolic compounds from the hydro distilled residual leaves and consequently their antioxidant activity. These results suggest that enzyme pre-treatment could be useful for extracting valuables components, and hold good potential for use in food, cosmetic and pharmaceutical industries.

An emerging body of evidence indicates that oleuropein, a biophenol usually found in olive leaves, extra-virgin olive oil and in some species of the Oleaceae family has potent biological and pharmacological properties. Its main pharmacological activities such as anticancer, cardioprotective, neuroprotective, gastroprotective, hepato-protective, anti-diabetes, anti-obesity and radioprotective, among others, are in large part attributed to its putative antioxidant and anti-inflammatory effects. This mini-review collects and discusses the scattered data available in the literature concerning oleuropein and/or oleuropein-rich extracts and highlights its chemistry, biosynthesis, biological activities and its possible mechanisms of action.

International audience; A phytochemical investigation of Diplotaxis virgata D.C. and D. erucoides (L.) D.C. (Brassicaceae) offered to the isolation of two new flavonoids isorhamnetin-3-O--l-glucopyranoside (1) and rhamnetin-3,3'-di-O--d-glucopyranoside (2), respectively. Their structures have been elucidated from the extended spectroscopic methods, including 1D- and 2D-NMR, UV and mass spectrometry analysis and by comparison with literature data. The fatty acid composition of the hexane extracts of the two species was also investigated by using GC-MS. The antioxidant activity of ethanol, ethyl acetate, n-butanol extracts and the isolated compounds from the two species was evaluated using DPPH and ABTS(+) scavenging assays. All the tested samples showed an efficient radical scavenging ability, with IC50 values ranging from 16-40 mu g/mL for the DPPH and from 17-44 mu g/mL for the ABTS(+) assays. In addition, the antibacterial activity of the prepared extracts and compounds 1 and 2, determined by well diffusion agar method against two Gram positive and five Gram negative bacteria, was evaluated and the results showed significant effects against all strains used.

The chemical composition of a Cyperus rotundus methanol extract was investigated. The phenol content determined by the Folin–Ciocalteu method was 83.6 ± 5.42 mEGA.g-1 and the flavonoid content assayed by the AlCl3 method was 32.65 ± 3.5 mEQ.g-1. The phenolic composition determined by HPLC-DAD showed the presence of phenolic acids (chlorogenic, caffeic, ferulic, syringic acids) and flavonoids (luteolin, quercetin, apigenin, myricetin). The antioxidant activity of the extract was evaluated using the 1,1-diphenyl-2-picrylhydrazyl (DPPH.) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid)(ABTS.+) radical scavenging assays and the β-carotene bleaching test. The EC50 values were 5.76 ± 0.83 µg/mL and 18.08 ± 0.6µg/mL for DPPH. and ABTS.+, respectively. The antioxidant activity coefficient (AAC) was 670.8 ± 4.2. The antibacterial activity determined by the disc diffusion and submerged culture methods against four Gram negative and two Gram positive bacteria showed effects against all strains. Cytochrome P450 (CYPs) inhibitory activity was evaluated against CYP1A2, CYP3A4 and CYP2D6, which was the most inhibited (IC50 =11.13± 0.04µg/mL).Keywords: Cyperus rotundus, chemical composition, antioxidant activity, antimicrobial activity, cytochrome inhibition

Root essential oil of Pulicaria mauritanica Coss. (Asteraceae) collected from western Algeria was analysed using a combination of chromatographic (CC, GC/FID, GC(RI)] and spectroscopic [GC–MS, 13C-NMR] techniques. Thirty-eight compounds accounting for 90.4% of the whole composition were identified. The oil composition was dominated by thymyl derivatives (2,5-dimethoxy-p-cymene (37.2%), 6-methoxythymyl isobutyrate (14.2%), 10-isobutyryloxy-8,9-dehydrothymyl isobutyrate (4.8%) and thymyl isobutyrate (3.1%)), as well as by neryl isobutyrate (11.1%). A new natural compound was isolated and the structure was elucidated as 1S,2S,5S,8S-modhephan-3-one (relative stereochemistry). Copyright © 2014 John Wiley & Sons, Ltd.

International audience; The present work aims to investigate the maturation-related changes in phenolic profile of Melia azedarach (L.) leaves (young and old) and fruits (pulp and kernel) at two developmental stages. A total of 26 phenolic compounds were identified by high-performance liquid chromatography-diode-array detector-hyphenated with tandem mass spectromdtry (HPLC-DAD-ESI MS/MS). They include phenolic acids, flavonols and flavanols which were found mostly in glycosylated forms. The main phenolic compounds were found to be rutin (5.86-21.33%, of total integrated peak area at 280 nm), quercetin-3-O-neohesperidoside (3.95-8.76%), kaempferol-3-O-rutinoside (2.73-11.23%), feruloylglucaric acid (0.85-11.84%) and feruloylquinic acid derivative (1.94-11.07%). The pattern distribution of phenolic compounds was organ-specific, and somewhat variable depending on the stage of maturation. Additionally, the total phenol content was determined as well as the antioxidant capacity using different in vitro assays. The extracts of young leaves demonstrated the highest total phenol content (85.4 mg GAE/g extract), and exhibited the strongest scavenging activity against 2,2-diphenyl-1-picrylhydrazyl DPPH and the highest oxygen radical absorbance capacity ORAC (235 and 328 mg Trolox equivalents/g extract, respectively) compared to old leaves and immature/mature fruit parts. In contrast, the highest metal chelating activity (MCA) was observed in immature pulp extracts (22.85 mg EDTA equivalents/g extract). Pearson's correlation and principal component analysis (PCA) showed that quercetin-3-O-neohesperidoside, rutin and kaempferol-3-O-rutinoside were the main contributors on the antioxidant capacity. On the basis of these results, M. azedarach could serve as an excellent source of natural antioxidants which could be used for pharmaceutical and cosmeceutical applications.

Purpose The paper aims to analyse the effect of acid hydrolysis on the chemical composition and the biological activities of Rubia tinctorum collected from the south of Tunisia. It proposes to clarify the relationship between alizarin content and the antioxidant and antimicrobial activities of Rubia extract. Design/methodology/approach The paper opted for analytical tools (HPLC) and the in-vitro study of biological activities, namely, the antioxidant activity which is evaluated using the radical scavenging assay (ABTS) and ferric reducing power assay (FRAP); the antimicrobial activity is tested using the wells agar diffusion method. Findings The paper provides information about the positive effect of acid hydrolysis, namely, the enhancement of alizarin content in the extract which has increased its antioxidant and antimicrobial activities. Originality/value This paper fulfils an identified need to study the relationship between the chemical composition, biological activities and colour enhancement.

International audience; The chemical composition of Cyperus rotundus L. tubers essential oil from the South of Tunisia was analyzed using GC-FID and GC-MS. Fifty compounds were identified representing 84.6 % of the total oil. A new chemotype was found in Tunisia. This essential oil was characterized by sesquiterpenes abundance (78.3 %) mainly represented by cyperene (15.2 %) and cyperotundone (19.7 %). The essential oil (EO) was further fractionated into three fractions (F1: n-pentane, F2: n-pentane/diethyl ether (95/5) and F3: diethyl ether). The antioxidant activity of the EO and its fractions was tested using the 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging test and beta-carotene bleaching method. Results showed that the whole EO was more active than the fractions with an effective concentration (EC50) of 0.85 +/- 0.03 mg/mL and an antioxidant activity coefficient (AAC) of 396.0 +/- 2.4. The antimicrobial activity of the EO and its fractions was evaluated using the disc diffusion method against six foodborne pathogens and results showed that Staphylococcus aureus was the most inhibited bacterium with an inhibition diameter of 15.2 +/- 0.8 mm for the whole EO.

Air-, oven- and freeze-dried garlic bulbs were hydrodistilled and the resulting essential oils were analyzed by gas chromatography (GC) and GC/mass spectrometry (GC/MS). The highest yields were 0.6 and 0.5% (w/w) for freeze- and oven-dried samples, respectively. The essential oils were characterized by a high amount of sulfur compounds (84.3–98.9%) with diallyl trisulfide (37.3–45.9%), diallyl disulfide (17.5–35.6%) and methyl allyl trisulfide (7.7–10.4%) being the major components. Remarkable qualitative and quantitative differences between the investigated oils owing to the drying procedure were found and a set of marker components was established to differentiate between them.

International audience; Volatile oil constituents of Tunisian sweet orange (Citrus sinensis Osbeck) cv. Meski (MES), Valencia Late (VAL), Thomson Navel (THN) and Maltaise Blanc (MAB); mandarin (Citrus reticulate Blanco); sour orange (Citrus aurantium L cv. Amara (AM)) and pummelo (Citrus grandis Osbeck) were obtained by hydrodistillation and analysed by gas chromatography (GC) combined with a flame ionisation detector (FID) and mass spectrometry (MS). A total of 41 components accounting for more than 95% of the total essential oils were identified, and oxygenated monoterpenes (69.5-99.9%) were found as the most prominent fraction in all oil samples. The main constituents were linalool (3.1-73%), isoborneol (0-55.8%) and tepinen-4-ol (1.1-19.2%). A high degree of inter-and intraspecific chemical variability between species and cultivars was found to be genetically determined, and a set of distinctive traits (chemical markers) in the essential oils profile was established. Principal component analysis (PCA) and hierarchical cluster analysis (HCA) of all identified components grouped the oils into two main chemotypes (linalool/isoborneol and isoborneol/linalool).

International audience; A comprehensive study on the volatile oil and phenolic constituents of Ailanthus altissima Swingle (Simaroubaceae) leaves was performed. Methanolic extracts of leaves and their hydrodistilled residues were screened for their antioxidant, antimicrobial and phytotoxic properties. The results showed that the leaf volatile oils were a complex mixture of more than a hundred components, mainly composed by non-terpenic compounds (tetradecanol, heneicosane, tricosane and docosane) and sesquiterpene hydrocarbons (α-curcumene and α-gurjunene). Methanolic extracts from leaves contain the highest level of total phenolic content, while those from the hydrodistilled residues showed the highest total flavonoid content. The most frequent phenolic compounds identified by HPLC-DAD-MS were gallic acid, chlorogenic acid, HHDP-galloylglucose, epicatechin, rutin, hyperoside and quercetin-3-galloyl hexoside. Evaluation of the antioxidant activities by using four complementary tests (DPPH, ABTS, 2-deoxyribose and FRAP) showed that both extracts exhibited strong concentration-dependent antioxidant activities. These extracts were efficient against Gram-positive bacteria, but not active against Gram-negative bacterial strains and the yeast Candida albicans. They also exhibited strong inhibitory effects on the germination and the radicle growth of the wild Daucus carota. This work provides scientific supports for the high antioxidant and phytotoxic activities of this species and thus, it may find potential applications in the development of natural herbicides and antioxidants for agro-food and pharmaceutical industries.

International audience; The main goal of the present study is to evaluate the effects of enzymatic pre-treatment on the yields, chemical composition and antimicrobial activities of the essential oils of Thymus capitatus and Rosmarinus officinalis leaves. In T. capitatus, application of cellulase, hemicellulase and combination of both enzymes induced 63.55, 23.72 and 109% increase in the essential oil yields. It also induced increment by 2.7, 31 and 38% in the amount of its main component carvacrol. In R. officinalis, enzymatic treatment resulted in enhanced oil yields by 5, 50 and 20% for cellulase, hemicellulase and the combination of both enzymes, respectively. In contrast to T. capitatus, the amount of the main component 1,8-cineole dropped by 17.73, 36.92 and 15.46% in oils extracted from cellulase, hemicellulase and cellulose/hemicellulase treated samples of R. officinalis. At the same time, the essential oils (at 1/32 and 1/4 dilution for T. capitatus and R. officinalis, respectively) were evaluated for their antimicrobial activities against 6 food-borne pathogens (Escherichia coli, Salmonella typhimurium, Streptococcus agalactiae, Staphylococcus aureus, Enterococcus feacium and Candida albicans). All investigated oils exhibited antimicrobial activity with those issued from hemicellulase treated samples being the most effective. Enzymatic pre-treatment could be useful for enhancing yield and antimicrobial activity of the essential oils, and hold a good potential for use in food and pharmaceutical industries

International audience; A reliable database is established from the analysis of 500 French royal jellies (RJ). Diversity of geographical origins, harvesting seasons, and forage sources were taken into account. Authenticity intervals for numerous physicochemical parameters have been established from French RJs, obtained without bee-feeding with artificial sugars or proteins. RJs from Italy and non-European countries, derived from feeding experiments, were analysed and compared with the database. Differences in 10-HDA, d13C and sugars (sucrose, erlose, maltose, maltotriose) contents were observed. Sucrose and erlose contents in French RJs were less than 1.8 and 0.4%, respectively, whereas they attained 3.9 and 2.0% in some commercial samples and 7.7 and 1.7% in RJs produced by sugarcane feeding. Maltose and maltotriose contents were less than 1.0 and 0.2% in French RJs, and they can attain levels of 2.6 and 0.4% in commercial samples; they can be as high as 5.5 and 1.7% in RJs obtained by bee-feeding with starch hydrolysate syrups. RJs obtained with and without feeding exhibit d13C values ranging from 26.45 to 23.73%, and from 26.05 to 14.65%, respectively. This study could be used to discriminate different production methods and provide a useful tool for identifying unknown commercial RJs. Highlights A total of 750 royal jellies (RJs) from different origins were studied. Origins included domestic, imported, obtained by bee-feeding. French RJ samples were chemically characterised. Authenticity intervals were calculated for authentic RJs. Sucrose, erlose, maltose, maltotriose and δ13C contents are bee-feeding markers.

We gratefully acknowledge Professor Genevieve Casanas for her scientific support in Statistical analysis. We also thank Dany Maitre for her excellent help in the identification of volatile constituents.; International audience; The composition of essential oil is known to depend on intrinsic and extrinsic factors, including season harvest and climate condition among others. Experiments were conducted to study the variation in the essential oil composition of Aristolochia longa ssp. paucinervis harvested at different period (August, 2009; September, 2011; March, 2012; and April, 2013). The essential oil composition was assessed by GC-FID and GC MS analyses, which revealed the presence of 103 molecules. Hence, samples collected in April 2013 showed the most complex composition (51 compounds) when compared with those collected in September 2011 (42 compounds), August 2009 (37 compounds) and March 2012 (35 compounds). Further, oxygenated sesquiterpenes (50.2-81.1%) and oxygenated monoterpenes (5.9-28.0%) are the major chemical groups.The antimicrobial properties of essential oils were evaluated against six microorganisms by the disc diffusion method. The highest activity is observed against all the Gram-positive bacteria. Increasingly, the essential oil isolated from roots collected in September (2011), exhibited the highest antimicrobial activity against Streptococcus agalactiae and Enterococcus faecium