Nitrogen compounds and polysaccharides changes during the biological ageing of sherry wines

Biologically aged sherry wines are elaborated by the so called “criadera” and “solera” system, which essentially involves development of the yeast on the wine surface forming a film velum for several years. In this work, a study on the changes that take place in polysaccharide and nitrogen compounds during the elaboration of sherry wines has been undertaken. The evolution of monosaccharides derived from polysaccharides as well as of amino acids and polypeptides have been investigated in wine samples at different stages of the elaboration process (young wines, “sobretablas”, “criaderas” and “solera”). Mannose, galactose, glucose and arabinose were detected in all analyzed wines; mannose being the most abundant carbohydrate, particularly in wines that aged longer. Glucose and galactose content also increased during the biological ageing of these wines, whereas arabinose concentration lowered during all period. Nitrogen compounds experimented a decrease and even some amino acids were not detected at the end of the ageing. Considering the increase in mannose and the decrease in amino acid levels, it is presumable that autolysis and growth of yeast occur at the same time during the elaboration of the sherry wines.     

Ultraviolet–visible spectroscopy and pattern recognition methods for differentiation and classification of wines

The feasibility of developing a qualitative model based on cheap and simple instrumentation to differentiate and classify wines from the apellation d’origine “La Mancha” (Spain) has been studied. The criteria for discrimination were origin, grape variety and ageing process. Ultraviolet–visible spectroscopy was used for the development of a inexpensive and simple screening approach. Once spectra were collected, a data exploratory analysis was carried out in order to both show trends hidden in the data matrix from the sample spectra and study the characteristics of the models thus developed. Principal components analysis and soft independent modelling of class analogy were used for the exploratory analysis and the development of classification models, respectively. The ultraviolet region has for the first time been used for the discrimination of types of wines. This region is of great importance for differentiation of wines according to both origin within a same apellation d’origine and ageing process. The sum of false positives and false negatives – the criteria used for evaluating errors – were not higher than 25%, and the classification of wines according to the origin zone yielded the best values (10%). Sample preparation was not necessary.     

Employment of near infrared spectroscopy to determine oak volatile compounds and ethylphenols in aged red wines

The aim of this work was to study the ability of NIR spectroscopy to determine oak volatile compounds and ethylphenols levels in aged red wines. For this purpose 510 wines aged with different storage time and in different oak barrel types were analyzed. Calibration models were developed from SBSE-GC–MS and NIR data using partial least squares (PLS) regression. In order to validate the calibration, full cross validation was employed. Results showed that the calibration statistics were very good (R² > 0.86) for all the compounds studied. In wines aged in French and in American and French oak barrels, and in “reserva” and “gran reserva” wines, the residual predictive deviation (RPD) obtained was higher than 1.5 in all the compounds and it was higher than 2 in some of the cases. In conclusion, near infrared spectroscopy can be used as a rapid tool to determine oak volatile compounds and ethylphenols in aged red wines.     

In-situ Iberian pig carcass classification using a micro-electro-mechanical system (MEMS)-based near infrared (NIR) spectrometer

Iberian pig (IP) products are gourmet foods highly appreciated at international markets, reaching high prices, because of its exquisite flavors. At present, there aren't practical and affordable analytical methods which can authenticate every single piece put on the market. This paper reports on the performance of a handheld micro-electro-mechanical system (MEMS)-based spectrometer (1600-2400 nm) for authentication-classification of individual IP carcasses into different commercial categories. Performance (accuracy and instrumental design) of the instrument was compared with that of high-resolution NIRS monochromators (400-2500 nm). A total of 300 carcasses of IPs raised under different feeding regimes (“Acorn”, “Recebo” and “Feed”) were analyzed in three modes (intact fat in the carcass, skin-free subcutaneous fat samples and melted fat samples). The best classification results for the MEMS instrument were: 93.9% “Acorn” carcasses correctly classified, 96.4% “Feed” and 60.6% “Recebo”, respectively. Evaluation of model performance confirmed the suitability of the handheld device for individual, fast, non-destructive, low-cost analysis of IP carcasses on the slaughterhouse line.     

Effect of the modifier (Graciano vs. Cabernet sauvignon) on blends of Tempranillo wine during ageing in the bottle. II. Colour and overall appreciation

The effect of Graciano (GRA) (Spanish valuable variety of limited production) vs. Cabernet Sauvignon (CS) (world-wide known French variety) on the colour of wines from Tempranillo (TEM-base wine) (largely cultivated Spanish variety), was studied in wine blends prepared with 25% and 10% (v/v) of each modifier after 4, 6, 9, 16.5 and 23 months of ageing in the bottle. Although possessing pH values very similar to the base wine, the blends of TEM with GRA or CS wines showed chromatic changes (higher a*, C*, CI, %red and %dA, and lower h, %yellow, tint and L*) that were perceptible by the human eye, even when using as little as 10% of modifier wine. However, no differences in colour parameters were found between the TEM-GRA (90:10) and the TEM-CS (90:10) blends, and between the TEM-GRA (75:25) and the TEM-CS (75:25) ones, this being consistent with the results relating to the temporal evolution of anthocyanins and flavanols (Part I). Moreover, the results of the principal component analysis indicated that the degree of interrelation existing between the colour parameters and the phenolic components during ageing in the bottle was similar for the TEM-GRA and TEM-CS blends. From a practical point of view, the ANOVA analysis also demonstrated that for any of the modifier wines used, certain colour parameters and phenolic components allowed differentiation between the base wine and the 75:25 blends, whereas others allowed differentiation between the base wine and both the 90:10 and 75:25 blends, during the ageing period studied. Some similarities between GRA and CS as modifier wines of TEM blends were also found in terms of their organoleptic characteristics, also demonstrating that both varieties could render blended wines with better overall quality attributes than the base wine after 23 months of ageing in the bottle.     

Chemical composition and functional properties of Ulva lactuca seaweed collected in Tunisia

The chemical composition and some functional properties of the dried “Ulva lactuca” algae, collected from the littoral between the Taboulba and Sayada area, were determined. The dried “U. lactuca” algae were investigated for their soluble, insoluble and total dietary fibre content, mineral amount, amino acid and fatty acid profiles, swelling capacity (SWC), water holding capacity (WHC) and oil holding capacity (OHC). Results showed that “U. lactuca” alga powder was characterised by a high content of fibres (54.0%), minerals (19.6%), proteins (8.5%) and lipids (7.9%). The neutral fibres contain hemicellulose (20.6%), cellulose (9.0%) and lignin (1.7%). The proteinic fraction analysis indicated the presence of essential amino acids, which represent 42.0% of the total amino acids. The fatty acids profile was dominated by the palmitic acid, which represents about 60.0% of the total fatty acids, followed by oleic acid (16.0%). The study of the functional properties proved that SWC, WHC and OHC of this alga varied with temperatures and that were comparable to those of some commercial fibre rich products.     

Biogenic amine content of red Spanish wines: comparison of a direct ELISA and an HPLC method for the determination of histamine in wines

Biogenic amines were determined in 61 commercial red Spanish wines from various winemaking areas and elaborated with different vinification/ageing procedures. Biogenic amines (histamine, methylamine, ethylamine, tyramine, phenylethylamine, putrescine and cadaverine) analysis was carried out by RP-HPLC with o-phthaldialdehyde precolumn derivatization and fluorescence detection. Overall, histamine and putrescine were the most prevalent amines, being present in 75% and 71%, respectively, of the wines, followed by tyramine (56% of the wines). There were no significant differences between biogenic amine levels and ageing characteristics of the wines tested. Moreover, it was found that amines suspected to cause toxicological effects (histamine, tyramine and phenylethylamine) are no cause for concern in these Spanish wines as they are present in amounts well below the limit considered as physiological. A commercial competitive direct ELISA immunoassay method specific for the detection of histamine has also tested on these wines and the results were compared with the RP-HPLC method. Both methods showed a good agreement for histamine analysis of wines.     

Study of the counts,species and characteristics of the yeast population during the manufacture of dry-cured “lacón”. Effect of salt level

The aim of this work was to study the yeast population during the manufacture of dry-cured “lacón” (a Spanish traditional meat product) and the effect of the salting time. For this study, six batches of “lacón” were manufactured with three different salting times (LS (3 days of salting), MS (4 days of salting) and HS (5 days of salting)). Yeast counts increased significantly (P < 0.001) during the whole process from 2.60 to 6.37 log cfu/g. An increased length of salting time did not affect yeast counts throughout the manufacture of dry-cured “lacón”, although the highest yeast counts were obtained from LS batches. A total of 226 isolates were obtained from dry-cured “lacón” during drying-ripening stage, of which 151 were yeasts and were identified at the species level using molecular techniques. The total of 151 identified yeasts belonged to 4 different genera: Debaryomyces, Candida, Cryptococcus and Rhodotorula. Debaryomyces hansenii was the most abundant species isolated throughout the whole process as much in the interior as in the exterior of the pieces of three salt levels of “lacón” studied, while Candida zeylanoides was only isolated from the interior of MS and HS batches and from the exterior of LS and HS groups, but at lesser proportion than D. hansenii.     

Stilbene levels and antioxidant activity of Vranec and Merlot wines from Macedonia: Effect of variety and enological practices

The content of the stilbenes trans-resveratrol and piceid as well as the antioxidant activity of Macedonian red wines from the two main grape varieties Vranec and Merlot have been evaluated. Тhe effects of time of maceration, type of yeast and the level of sulphur dioxide applied on stilbene content and antioxidant activity have been studied. The most important factor in winemaking technology is the maceration time since the highest concentrations of trans-resveratrol, piceid and highest antioxidant activity were found following 6 and 10 days of maceration. Concerning the yeast type, higher concentrations of trans-resveratrol and piceid have been obtained with French yeast “Levuline CHP” in comparison to Macedonian yeast “Vinalco”. In contrast, the higher antioxidant activity of wines from both varieties of grapes was observed by application of Macedonian yeast “Vinalco”.     

Indigenous yeast population from Georgian aged wines produced by traditional “Kakhetian” method

The yeast microbiota present in wines produced by the ancient “Kakhetian” method in Georgia (EU) was studied. This technique involves the use of terracotta vessels (amphoras), during spontaneous fermentation, maceration phase and wine ageing. The analysed yeasts were collected from wines after maturation for one year in ten amphoras from a Georgian winery. The 260 isolates were all identified as Saccharomyces cerevisiae, and the majority were classified as flor yeasts by restriction analysis of ITS region. A first technological and molecular screening was used to select 70 strains for further characterization. Both genetic and metabolic characterization discriminated flor from non-flor strains. The combined results obtained by analysis of interdelta region and mtDNA-RFLP yielded 23 different biotypes; no biotype was common to flor and non-flor strains. The wines produced by flor yeasts showed a high content in acetaldehyde, acetic acid, acetoin, whereas the level of other compounds was similar to wines obtained by non-flor strains. This study represents the first report on the composition of yeast microbiota involved in the maturation of this traditional wine. These flor strains represent an interesting yeast population, in possession of peculiar characteristics allowing them to survive during wine ageing, becoming the dominant flora in the final wine.     

Classification of Brazilian honeys by physical and chemical analytical methods and low field nuclear magnetic resonance (LF H NMR)

This study evaluated the possibility of differentiating the botanical origin of honeys using Low Field Nuclear Magnetic Resonance (LF ¹H NMR). Eighty samples of honey from 8 different botanical sources (eucalyptus, “assa-lipto”, oranges, Barbados cherry, cashew tree, “assa-peixe”, “cipó-uva” and polyfloral) were analyzed. A close correlation (p < 0.01) was established between the LF ¹H NMR analysis and physical and chemical measurements, including water content, water activity, pH and color. Bi-exponential fitting of the transverse relaxation (T₂) data revealed two water populations in all samples, T₂₁ and T₂₂, corresponding to relaxation times of 0.6–1.8 ms and 2.3–5.4 ms respectively. The observed differences in the relaxation times suggest that these were influenced by the differences in botanical origins. Good linear correlations were observed between the T₂ and T₂₁ parameters and the physical and chemical data. This study demonstrated that LF ¹H NMR can be a viable technique for use in classifying honeys by their botanical origin.     

Proton NMR transverse relaxation measurements to study water dynamic states and age-related changes in Mozzarella di Bufala Campana cheese

Proton transverse magnetization decay curves of Mozzarella di Bufala Campana samples were measured and analysed for the presence in the sample of four components, namely “serum water”, “entrapped water”, “junction zone water” and “fat”, characterised by different transverse relaxation times, T₂. T₂ values were interpreted on the basis of the diffusive and chemical exchange model that allowed information to be obtained on the size of diffusive domains and dynamics of the water molecules. Furthermore, T₂ values were measured as a function of the aging time of Mozzarella samples, as produced by different cheese-makers. A decrease of “serum water” T₂ value with aging time was found and this may be used to monitor the evolution of Mozzarella samples up to seven days after manufacture.     

Traceability of olive oil based on volatiles pattern and multivariate analysis

An automated head-space solid-phase microextraction (HS-SPME)-based sampling procedure, coupled to gas chromatography–ion trap mass spectrometry (GC–ITMS), was developed and employed for fast characterisation of olive oil volatiles. In total, 914 samples were collected, over three production seasons, in north-western Italy—Liguria (n = 210) and other regions—in addition to the rest of Italy, Spain, France, Greece, Cyprus, and Turkey (n = 704) with the aim to distinguish, based on analytical (profiling) data, the olive oils labelled as “Ligurian” (protected denomination of origin region, PDO) from all the others (“non-Ligurian”). For the chemometric analysis, linear discriminant analysis (LDA) and artificial neural networks with multilayer perceptrons (ANN-MLP) were tested. Employing LDA, somewhat lower recognition (81.4%) and prediction (61.7%) abilities were obtained. The classification model was significantly improved using ANN-MLP. Under these conditions, the recognition (90.1%) and prediction (81.1%) abilities were achieved. The diagnostic value of the data obtained by one-dimensional GC–ITMS were compared with those generated by two-dimensional gas chromatography–time-of-flight mass spectrometry (GC × GC–TOFMS), allowing a comprehensive analysis of olive oil volatiles.     

Fatty acid compositions of selected varieties of Spanish dry ham related to their nutritional implications

Five varieties of Spanish dry cured ham were studied to assess their nutritional value in relation to fatty acids. Ten hams of the Traditional Speciality Guaranteed (TSG) “Jamón Serrano”, and the Protected Designations of Origin (PDO) “Jamón de Teruel”, “Dehesa de Extremadura”, “Jamón de Huelva” and “Guijuelo”, were analysed. Iberian hams (“Dehesa de Extremadura”, “Jamón de Huelva” and “Guijuelo”) were characterised by a lower proportion of saturated fatty acids (SFA) and a significantly higher percentage of monounsaturated fatty acids (MUFA) than white hams (“Jamón Serrano” and “Jamón de Teruel”). The Iberian varieties also showed a high proportion (approximately 50%) of C18:1 n − 9, while “Jamón Serrano” showed the highest percentage of C18:2n−6. The PUFA/SFA (P/S) ratio of the five varieties was ? 0.19, with the highest ratio corresponding to “Jamón Serrano” (0.3). The n−6/n−3 ratio was in the order of 13/1 in “Jamón Serrano” and “Jamón de Huelva”, and ranged from 9.3/1 to 10.3/1 in the other varieties. The most favourable hypocholesterolemic/Hypercholesterolemic (h/H) ratio (?2.5) was found in the Iberian varieties. TSG “Serrano” was shown to supply the lowest percentage of the recommended daily intake of MUFA, the Iberian varieties showed the highest percentage of the daily intake of long-chain PUFA, and PDO “Dehesa de Extremadura” showed the highest percentage of the intake of C18:3n−3. The higher MUFA proportion and h/H ratio observed in the Iberian hams, together with their contribution to the recommended daily intake of fatty acids, would make these products more suitable for healthier diets, although consumption must be recommended in moderation.     

Melissopalynological origin determination and volatile composition analysis of Corsican “chestnut grove” honeys

Fifty Corsican “chestnut grove” honeys were certified by melissopalynological analysis. Castanea sativa was strongly overrepresented and was accompanied mainly by Rubus sp., Quercus ilex, Anthyllis hermanniae, Myrtus communis, Genista sp., Erica arborea, Cistus creticus, and Fraxinus ornus. Headspace solid-phase microextraction was performed to investigate the volatile composition of Corsican chestnut catkins and chestnut grove honeys. The main compounds of the chestnut catkins were acetophenone (21.5%), methyl salicylate (13.4%), nonanal (10.9%), and linalool (7.5%), whereas the major constituents of the honeys were 2-aminoacetophenone (11.4%), benzaldehyde (10.8%), acetophenone (7.0%), nonanoic acid (5.9%), octanoic acid (5.0%), and 3-furaldehyde (4.9%). By entering the aromatic intensity, the relative frequency of C. sativa, Rubus sp., and A. hermanniae pollens, and the physicochemical parameters as discriminate variables, principal component analysis (PCA) and cluster analysis (CA) showed that the distribution of Corsican “chestnut grove” honeys correlates with climatic events and/or honeybee foraging behaviours.     

4-Ethylphenol and 4-ethylguaiacol depletion in wine using esterified cellulose

The ability of cellulose acetate, cellulose acetate propionate (CAP), cellulose acetate butyrate and cellulose propionate (CP) fibres to reduce 4-ethylphenol and 4-ethylguaiacol, causing the off-flavour named “Brett character”, was studied. CAP and CP performed best in a preliminary comparative test. The former was chosen because of its more favourable FDA classification for food contact substances. CAP effectiveness was studied in relation to the reduction in volatile phenols with doses of up to 20 g/l and wine contact times of up to 60 min. Using 4 g/l, reduction of both phenols was, on average, 31–32% in defective red wines. Wine treatment affected neither colour nor total proanthocyanidins and catechins, and wines were judged to be better than the corresponding spoiled controls. CAP fibre can be regenerated by washing with ethanol or aqueous solution (pH 12), without notable changes in depletion efficiency. The technological characteristics of CAP and, to a lesser extent, CP offer interesting prospects for producing filtration beds, pads and membranes for the treatment of wines and beverages affected by “Brett character”.