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- Development of headspace solid-phase microextraction-gas chromatography–mass spectrometry methodology for analysis of terpenoids in Madeira winesPublication . Câmara, J. S.; Alves, Maria Arminda; Marques, J. C.
- Changes in volatile composition of Madeira wines during their oxidative ageingPublication . Câmara, J. S.; Alves, Maria Arminda; Marques, J. C.The influence of the age in the volatile composition of Madeira wines made with Boal, Malvazia, Sercial and Verdelho varieties and aged in oak barrel during 1, 11 and 25 years old was been studied. For this purpose, the evolution of volatile compounds: higher alcohols, ethyl esters, fatty acids, furan compounds, enolic compounds, γ-lactones, dioxanes and dioxolanes, of the four most utilised varieties were determined using liquid–liquid extraction with dichloromeihane. Octan-3-ol was used as internal standard. The wines made with these varieties showed great differences in sugar content and small variations on pH and alcoholic degree. The results show that during ageing, the concentration of fatty acids ethyl esters, acetates and fatty acids decrease significantly contrarily to the great increase of ethyl esters of diprotic acids. There is a strong correlation between sotolon, 2-furfural, 5-methyl-2-furfural, 5-hydroxymethyl-2-furfural and 5-ethoxymethyl-2-furfural with wine ageing. These findings indicate that these compounds can be used as ageing wine markers. Among the molecules studied, sotolon [3-hydroxy-4,5-dimethyl-2(5H)-furanone] was one of the few molecules present in concentrations above the perception threshold in Madeira wines. 5-Eihoxymethyl-2-furfural formed from 5-hydroxymethyl-2-furfural and 2-furfural, derived from sugars, are also involved in the aroma of sweet fortified white wines aged in oxidative conditions. The sensory properties change significantly after long periods of conservation.
- Evaluation of the feasibility of the electronic tongue as a rapid analytical tool for wine age prediction and quantification of the organic acids and phenolic compounds. The case-study of Madeira winePublication . Rudnitskaya, A.; Rocha, S. M.; Legin, A.; Pereira, V.; Marques, J. C.A set of fourteen Madeira wines comprising wines produced from four Vitis vinifera L. varieties (Bual, Mal vasia, Verdelho and Tinta Negra Mole) that were 3, 6, 10 and 17 years old was analysed using HPLC and an electronic tongue (ET) multisensor system. Concentrations of 24 organic acids, phenolic and furanic compounds were determined by HPLC. The ET consisting of 26 potentiometric chemical sensors with plasticized PVC and chalcogenide glass membranes was used. Significance of the effects of age and vari ety on the ET response and wine composition with respect to the organic acids, phenolics and furanic derivatives were evaluated using ANOVA—Simultaneous Component Analysis (ASCA). Significance of the effects was estimated using a permutation test (1000 permutations). It was found that effects of age, grape variety and their interaction were significant for the HPLC data set and only the effect of age was significant for the ET data. Calibration models of the HPLC and ET data with respect to the wine age and of the ET data with respect to the concentration of the organic acids and phenolics were calculated using PLS1 regression. Models were validated using cross-validation. It was possible to predict wine age from HPLC and ET data with the accuracy in cross-validation of 2.6 and 1.8 years respectively. The ET was capable of detecting the following components (mean relative error in cross-validation is shown in the parentheses): tartaric (8%), citric (5%), formic (12%), protocatehuic (5%), vanillic (18%) and sinapic (14%) acids, catechin (6%), vanillin (12%) and trans-resveratrol (5%). The ET capability of predicting Madeira wine age with good accuracy (1.8 years) as well as quantify of some organic acids and phenolic compounds was demonstrated.
- Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatingsPublication . Câmara, J. S.; Marques, J. C.; Perestrelo, Rosa Maria de Sá; Rodrigues, F.; Oliveira, L.; Andrade, P.; Caldeira, M.A dynamic headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to ion trap mass spectrometry (GC–ITMS) method was developed and applied for the qualitative determination of the volatile compounds present in commercial whisky samples which alcoholic content was previously adjusted to 13% (v/v). Headspace SPME experimental conditions, such as fibre coating, extraction temperature and extraction time, were optimized in order to improve the extraction process. Five different SPME fibres were used in this study, namely, poly(dimethylsiloxane)(PDMS),poly(acrylate)(PA),Carboxen-poly(dimethylsiloxane)(CAR/PDMS),Carbowax-divinylbenzene(CW/DVB)and Carboxen-poly(dimethylsiloxane)-divinylbenzene (CAR/PDMS/DVB). The best results were obtained using a 75 m CAR/PDMS fibre during headspace extraction at 40◦C with stirring at 750rpm for 60min, after saturating the samples with salt. The optimised methodology was then appliedtoinvestigatethevolatilecompositionprofileofthreeScotchwhiskysamples—BlackLabel,BallantinesandHighlandClan.Approximately seventy volatile compounds were identified in the these samples, pertaining at several chemical groups, mainly fatty acids ethyl esters, higher alcohols, fatty acids, carbonyl compounds, monoterpenols, C13 norisoprenoids and some volatile phenols. The ethyl esters form an essential group of aroma components in whisky, to which they confer a pleasant aroma, with “fruity” odours. Qualitatively, the isoamyl acetate, with “banana” aroma,wasthemostinteresting.Quantitatively,significantcomponentsareethylestersofcaprilic,capricandlauricacids.Thehighestconcentration of fatty acids, were observed for caprilic and capric acids. From the higher alcohols the fusel oils (3-methylbutan-1-ol and 2.phenyletanol) are the most important ones.
- Screening of volatile composition from portuguese multifloral honeys using headspace solid-phase microextraction-gas chromatography–quadrupole mass spectrometryPublication . Pontes, Marisela; Marques, J. C.; Câmara, J. S.The volatile composition from four types of multifloral Portuguese (produced in Madeira Island) honeys was investigated by a suitable analytical procedure based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography–quadrupole mass spectrometry detection (GC–qMS). The performance of five commercially available SPME fibres: 100 μm polydimethylsiloxane, PDMS; 85 μm polyacrylate, PA; 50/30 μm divinylbenzene/carboxen on polydimethylsiloxane, DVB/CAR/PDMS (StableFlex); 75 μm carboxen/polydimethylsiloxane, CAR/PDMS, and 65 μm carbowax/divinylbenzene, CW/DVB; were evaluated and compared. The highest amounts of extract, in terms of the maximum signal obtained for the total volatile composition, were obtained with a DVB/CAR/PDMS coating fibre at 60 °C during an extraction time of 40 min with a constant stirring at 750 rpm, after saturating the sample with NaCl (30%). Using this methodology more than one hundred volatile compounds, belonging to different biosynthetic pathways were identified, including monoterpenols, C13-norisoprenoids, sesquiterpenes, higher alcohols, ethyl esters and fatty acids. The main components of the HS-SPME samples of honey were in average ethanol, hotrienol, benzeneacetaldehyde, furfural, trans-linalool oxide and 1,3-dihydroxy-2-propanone.
- Varietal flavour compounds of four grape varieties producing Madeira winesPublication . Câmara, J. S.; Herbert, Paulo; Marques, J. C.; Alves, Maria ArmindaBoal, Malvasia, Sercial and Verdelho are the main white grape varieties used in Madeira wine production. To estimate the free fraction of varietal aroma compounds of these varieties, 39 samples of musts were analysed to determine their content of monoterpenols and C13 norisoprenoids (terpenoids), using dynamic headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry. The r-values for linearity studies of the analytical method used, varied between 0.977 (nerolidol) and 0.999 (linalool). The repeatability for each compound varied between 2.5% (citronellol) and 11.8% (β-ionone). The mean values from three vintages (1998, 1999 and 2000) confirmed that these musts have differentiated contents of terpenoids. In opposition to Verdelho musts, Malvasia showed the highest free terpenoids content. In order to establish relations between the compounds and the varieties under investigation, principal component analysis and linear discriminant analysis were applied to the data, revealing a good separation and classification power between the four groups as a function of varietal origin.
- Heterocyclic acetals in Madeira winesPublication . Câmara, J. S.; Marques, J. C.; Alves, A.; Ferreira, A. C. SilvaThe maturation of Madeira wines usually involves exposure to relatively high temperatures which affect the aroma and flavour composition leading to the formation of the typical and characteristic bouquet of these wines. The formation of heterocyclic acetals (1,3-dioxanes and 1,3-dioxolanes) was investigated in order to determine levels and for possible use as indicators of wine age. The results show a linear correlation of the investigated acetals with wine age but suggest that the acetalization reaction is not particularly affected by the drastic oxidative conditions observed during maturation.
- Analytical characterization of the aroma of Tinta Negra Mole red wine: Identification of the main odorants compoundsPublication . Perestrelo, Rosa Maria de Sá; Fernandes, A.; Albuquerque, F. F.; Marques, J. C.; Câmara, J. S.A method for the simultaneous determination of major and minor volatiles composition in different types (dry, medium dry, sweet and medium sweet) of a young Tinta Negra Mole (TNM) monovarietal red wine from 2003 harvest has been validated. Wine samples preparation includes a dichloromethane liquid–liquid extraction followed by concentration under a nitrogen atmosphere. The extracted fraction was analysed by gas chromatography–mass spectrometry and give quantitative information for more than 86 analytes whose concentration range from few μg l−1 to 259.1 mg l−1. The method enables high recovery of volatile compounds in wine good linearity with (r2) values higher than 0.980 and good sensitivity. The limits of detection range from 0.003 to 0.534 mg l−1 and limits of quantification from 0.009 to 1.170 mg l−1. The method allows satisfactory determination of more than 80 compounds in the TNM red wines. These wines are characterized by a high content of higher alcohols, ethyl esters, fatty acids and lactones. The levels of sulphur compounds in Tinta Negra Mole medium sweet wines are very low, but they have the highest concentration of carbonyl compounds. Quantitative analysis of the main odorants followed by the determination of aroma index allow us elucidate the aroma of these varieties. On the basis of their odour description and odour threshold, the most powerful odorants of Tinta Negra Mole wines were tentatively established.
- Impact of forced-aging process on Madeira Wine flavorPublication . Silva, Hugo Oliveira e; Pinho, Paula Guedes de; Machado, Beatriz P.; Hogg, Tim; Marques, J. C.; Câmara, José S.; Albuquerque, F. F.; Ferreira, António C. SilvaThe aim of this study was to determine the optimal temperature and baking time to obtain a Madeira wine considered typical by an expert panel. For this purpose simultaneous descriptive analyses of typical Madeira wines were performed, and seven descriptors were selected: “dried fruit”, “nutty”, “musty”, “baked”, “oak”, “mushroom”, and “brown sugar”. Up to 10 odor-active zones were the most frequently cited by the members of the GC-olfactometry panel as corresponding to the panel’s descriptors. The odor importance of each of the zones reported by the GC-O analysis was ranked by AEDA. Three odor zones were identified as common to both Malvasia and Sercial wines and had retention indices (RI) of 1993 (“brown sugar” and “toasted”), 2151 (“brown sugar”), and 2174 (“nutty”, “driedfruits”);sotolonwasidentifiedasresponsibleforthislastaroma.Severalmoleculeswereselected to be quantified on baked wines on the basis of AEDA results and expected Maillard volatiles, such as sotolon, furfural, 5-methylfurfural, 5-ethoximethylfurfural, methional, and phenylacetaldehyde. It was observed that typicity scores were positively correlated with the concentrations of sotolon and sugar and baking time and negatively with the fermentation length.
- Simultaneous analysis of free amino acids and biogenic amines in honey and wine samples using in loop orthophthalaldeyde derivatization procedurePublication . Pereira, Vanda Nulita Gomes; Pontes, Marisela; Câmara, J. S.; Marques, J. C.This work presents a RP-HPLC method for the simultaneous quantification of free amino acids and biogenic amines in liquid food matrices and the results of the application to honey and wine samples obtained from different production processes and geographic origins. The developed methodology is based on a pre-column derivatization with o-phthaldialdehyde carried out in the sample injection loop. The compounds were separated in a Nova-Pack RP-C18 column (150 mm × 3.9 mm, 4 μm) at 35 °C. The mobile phase used was a mixture of phase A: 10 mM sodium phosphate buffer (pH 7.3), methanol and tetrahydrofuran (91:8:1); and phase B: methanol and phosphate buffer (80:20), with a flow rate of 1.0 ml/min. Fluorescence detection was used at an excitation wavelength of 335 nm and an emission wavelength of 440 nm. The separation and quantification of 19 amino acids and 6 amines was carried out in a single run as their OPA/MCE derivatives elute within 80 min, ensuring a reproducible quantification. The method showed to be adequate for the purpose, with an average RSD of 2% for the different amino acids; detection limits varying between 0.71 mg/l (Asn) and 8.26 mg/l (Lys) and recovery rates between 63.0% (Cad) and 98.0% (Asp). The amino acids present at the highest concentration in honey and wine samples were phenylalanine and arginine, respectively. Only residual levels of biogenic amines were detected in the analysed samples.