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Morinda citrifolia is a plant that grows in Brazilian northeast and presented a wide range of therapeutic, industrial and technological applications. Based on this, the aim of this work was to study the chemical composition, main biological activities and potential toxicity of its extracts, aiming their industrial application. Important compounds were identified in the methanolic extracts obtained by ultrasonic and Soxhlet extractions from leaves and fruits. GC × GC allowed for the identification of phytosterols, fatty acids and methyl esters, besides others (scopoletin, hydrocarbons, alcohols, terpenes). By HPLC-DAD, compounds like catechin, rutin, quercetin could be also identified and quantified. Their content of polyphenols and flavonoids was considered between the international standards. The extracts showed high antioxidant activities (EC50 ∼ 300 µg mL-1, using DPPH assay) compared with those from the literature. The extracts did not show toxicity or mutagenicity, but presented cytotoxicity, which can indicate their use safely in phytotherapic or nutritional applications.

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Abstract The potential of the biome caatinga (exclusive from northeastern Brazil) has been evaluated in recent research for application in the pharmaceutical industry. Among the species of medicinal plants from caatinga, one can highlight the Commiphora leptophloeos (umburana), which has been used as infusions and syrups by the regional population for inflammatory and infectious diseases. Essential oils from umburana leaves and barks were obtained in a Clevenger apparatus and analyzed by gas chromatography/mass spectrometry, and total phenolic and flavonoids were determined by spectrophotometric analysis. It was observed that a large part of the major compounds present in the essential oil is described as having antitumor activity, enabling research in investigational oncology with umburana (C. leptophloeos). In addition, some little explored components have been identified, such as cadinene, alpha-selinene, and elemenone. Despite being easily found in several plants, there are no clinical trials involving their biological activity in a well-defined isolated form, which could make exploring new studies possible. Furthermore, the presence of phenolic compounds and flavonoids allows future studies about the potential antimicrobial and antioxidant activity.

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Phenolic compounds of the first and second racking wine lees, including anthocyanins, were qualitatively and quantitatively analyzed by HPLC-DAD-MS. Wine lees from both rackings displayed similar chromatographic profiles. Therefore, it was impossible to differentiate the qualitative results regarding phenolic compounds. On the other hand, those from the second racking presented, on average, concentration of polyphenols twice as high. While the ones from the first racking displayed ca. 1600 mg phenolic compounds and 400 mg anthocyanins per kg of dry matter, those from the second racking have shown ca. 3300 mg phenolic compounds and 700 mg anthocyanins per kg of dry matter. These outcomes indicate that, although the wine lees from the first racking can be employed as a resource for phenolic compounds recovery, those from the second racking are more appropriate for this purpose.

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Bio-oils were produced through intermediate (IP) and fast pyrolysis (FP), using Eucalyptus sp. (hardwood) and Picea abies (softwood), wood wastes produced in large scale in Pulp and Paper industries. Characterization of these bio-oils was made using GC/qMS and GC×GC/TOFMS. The use of GC×GC provided a broader characterization of bio-oils and it allowed tracing potential markers of hardwood bio-oil, such as dimethoxy-phenols, which might co-elute in 1D-GC. Catalytic FP increased the percentage of aromatic hydrocarbons in P. abies bio-oil, indicating its potential for fuel production. However, the presence of polyaromatic hydrocarbons (PAH) draws attention to the need of a proper management of pyrolysis process in order to avoid the production of toxic compounds and also to the importance of GC×GC/TOFMS use to avoid co-elutions and consequent inaccuracies related to identification and quantification associated with GC/qMS. Ketones and phenols were the major bio-oil compounds and they might be applied to polymer production.

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This study reports, for the first time, the main changes that occur with some important aroma compounds of Moscatel sparkling wines during winemaking, measured using headspace solid-phase microextraction, one-dimensional and comprehensive two-dimensional gas chromatography (GC×GC) with mass spectrometry detection (MS). The best conditions of volatile extraction included the use of PDMS/DVB fibre, 2mL of wine, 30% of NaCl, 40°C for 30min. The chromatographic profile of sparkling wines showed decreasing amounts of monoterpenes (limonene, 4-terpineol, terpinolene, citronellol, α-terpineol, linalool, hotrienol, and nerol oxide), increasing amounts of esters (terpenyl esters, ethyl octanoate, ethyl decanoate and hexyl acetate) and alcohols (1-nonanol and 2-phenylethanol). Sixty-nine compounds co-eluted in the first dimension; only six co-eluted in the second dimension. GC×GC/TOFMS allows more detailed study of the volatile profile of sparkling wines.

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Zygosaccharomyces bailii BCV 08, a yeast isolated from red wine barrels in Brazil, was evaluated as co-starter in fermentations with Saccharomyces cerevisiae. Z. bailii BCV 08 was preliminarily shown to produce high levels of esters, and the production was optimized in bench and bioreactor scales using grape must. White wine vinifications were conducted with mixed cultures containing different proportions of Z. bailii BCV 08 and an enological strain of S. cerevisiae. In all trials that contained Z. bailii BCV 08, the production of ethyl esters was enhanced in comparison to the vinification control. Our results clearly show the potential of Z. bailii BCV 08 as a mixed starter with S. cerevisiae in order to increase the aromatic complexity of wine.

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The wood treatment process uses substances that generate hazardous compounds that may contaminate environmental compartments. In the present study, an area under influence of a deactivated wood treatment plant was investigated to evaluate past air pollution and to try to understand local air dispersion. Attic dust samples were collected from eight residences around the plant and from two residences outside this area, as reference samples. The presence of copper, chromium, arsenic, pentachlorophenol, sixteen priority polycyclic aromatic hydrocarbons and mutagenic activity using Salmonella/microsome assay was evaluated. The residences close to the entrance to the plant were the most affected, according to potentially toxic elements analysis. The PCP concentration was 0.49 mg/kg and the total PAHs content ranged from 0.40 to 13.31 µg/g with greater dispersion than potentially toxic elements. The highest mutagenesis values were 15,905 and 10,399 revertants/g of dust in the absence and presence of S9 mix (mammalian metabolic activation), respectively. Samples in which the total PAHs concentration was less than 2 µg/g no mutagenic effects were observed, including the residences in the reference area. The contribution of PAHs to mutagenesis was 10 percent, indicating that other compounds may contribute to the mutagenic effect. These results suggest that the population was or is potentially exposed to substances with strong effects on health.

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Separation of polycyclic aromatic sulfur heterocycles among themselves and also from interferents in petrochemical matrices is a challenging task because of their low concentration, matrix complexity, and also due to the presence of polyaromatic hydrocarbons, as they present similar physico-chemical properties. Therefore, the objective of this work was preparation, characterization, and application of a stationary phase for separation of these compounds in a heavy gas oil sample and their identification by comprehensive two-dimensional gas chromatography. The stationary phase was prepared by grafting mercaptopropyltrimethoxisilane onto a silica surface, followed by palladium(II) chloride immobilization. Elemental analysis, thermogravimetry, nitrogen adsorption-desorption isotherms, infrared analysis, and scanning electron microscopy were performed to characterize this solid phase. Sulfur compounds were separated in an open column packed with the stationary phase and analyzed by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection. The number of compounds tentatively identified was 314 and their classes were thiophenes, benzotiophenes, dibenzothiophenes, naphthothiophenes, benzonaphthothiophenes, and dinaphthothiophenes. Separation among sulfur compounds and polyaromatic hydrocarbons was successful, which is a difficult goal to achieve with the traditionally employed solid phases. Some recalcitrant compounds (dibenzothiophenes with substituents of two and four carbons) were fully separated and tentatively identified.

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The separation of the organic sulfur compounds (OSC) of petroleum or its heavy fractions is a critical step and is essential for the correct characterization of these compounds, especially due to similar physical and chemical properties of polycyclic aromatic sulfur heterocycles (PASH) and polycyclic aromatic hydrocarbons (PAH). This similarity results in coelutions among PAH and PASH and for this reason former steps of fractionation are required before gas chromatographic analysis. The objective of this study was to evaluate the potential of GC×GC for the separation and identification of OSC in a heavy gas oil sample without fractionation, after pre-fractionation in an alumina column and also after fractionation process. This last one was performed with a modified stationary phase manufactured and characterized in the laboratory, called Pd(II)-MPSG, where palladium is chemically linked to silica through mercaptopropyl groups. The fractions obtained from both procedures were analyzed by GC×GC/TOFMS, which was effective to separate and identify various classes of OSC. A hundred and thirty-five compounds were tentatively identified in the sample that was only pre-fractionated. However, when the fractionation was also performed with the Pd(II)-MPSG phase, a larger number of sulfur compounds were found (317). Results have shown that the analysis of a pre-fractionated sample by GC×GC/TOFMS is suitable when the goal is a general characterization of classes of compounds in the sample, while a more detailed analysis of PASH can be performed, using also the fractionation Pd(II)-MPSG phase. GC×GC/TOFMS played a major role in the comparison of samples obtained from pre-fractionation and fractionation steps due to its high peak capacity, selectivity, organized distribution of chromatographic peaks and resolution.

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ETHNOPHARMACOLOGICAL RELEVANCE: Bauhinia platypetala Burch. is a traditionally used Brazilian medicinal plant, although no evidence in the literature substantiates the safety of its use. AIM OF THE STUDY: The aim of this study was to investigate the safety of the ethanolic extract and the ethereal fraction of B. platypetala leaves. MATERIALS AND METHODS: The identification of chemical compounds from the B. platypetala ethanolic extract and its ethereal fraction was performed by GC/MS and ESI-MS/MS. The plant's toxicological, cytotoxic, mutagenic and genotoxic properties were determined in Saccharomyces cerevisiae strains and V79 cell culture by survival assays and comet assay. RESULTS: The major compound identified in the B. platypetala ethanolic extract is palmitic acid, kaempferitirin and quercitrin, while the B. platypetala ethereal fraction was found to be rich in phytol, gamma-sitosterol and vitamin E. Moreover, the results indicated that the B. platypetala ethanolic extract has an anti-oxidative effect against H(2)O(2) in yeast. In addition, the B. platypetala ethanolic extract did not induce mutagenic effects on the S. cerevisiae N123 strain, but the ethereal fraction of B. platypetala at higher concentrations (250-500 µg/mL) induced cytotoxicity and mutagenicity. A slight cytotoxic effect was observed in mammalian V79 cells; however, both the B. platypetala ethanolic extract and its ethereal fraction were able to induce DNA strand breaks in V79 cells, as detected by the alkaline comet assay. CONCLUSION: The B. platypetala ethanolic extract has antioxidant action and showed absence of mutagenic effects in yeast S. cerevisiae. On the other hand B. platypetala ethereal fraction is mutagenic and does not show antioxidant activity in yeast. In mammalian cells B. platypetala ethanolic extract and it's ethereal fraction induce cyotoxic and genotoxic action.

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