Formation of volatile and maturation‐related congeners during the aging of sugarcane spirit in oak barrels

The aging process of distilled spirits is a complex system based on the extraction of molecules from the wood and interactions with the liquid, the phenomenon of migration of wood constituents, as well as the formation and degradation of several compounds. Volatile and maturation‐related congeners were evaluated during the aging process of cachaça, a Brazilian sugarcane spirit aged in oak barrels. Aged cachaça presented alterations in the levels of ethanol, higher alcohols, acetaldehyde, volatile acidity, ethyl acetate, total volatile congeners, isoamyl alcohol, ethyl carbamate and copper. The aging markers (gallic acid, furfural, 5‐hydroxymethylfurfural, vanillic acid, syringic acid, vanillin, syringaldehyde, sinapaldehyde and coniferaldehyde) were compared with the compounds found in whisky, cognac, armagnac, bourbon and brandy. Monitoring the generation and evolution of congeners during the aging process allowed the characterization of cachaça and the identification of product maturity. Copyright © 2014 The Institute of Brewing & Distilling     

Maturation related phenolic compounds in cachaça aged in new oak barrels

Aging cachaça in wooden barrels improves its chemical and sensory profile and adds quality. Maturation of distilled spirits is influenced by factors such as the species of wood to make the barrels, degree of internal toasting, number of uses of the barrel and aging time. The level of maturation of distillates can be determined based on the concentration of age marker phenolic compounds extracted from the lignin of the wooden barrel, as well as their relationships with each other. This study characterises the aging process of cachaça by analysing the mechanism of lignin degradation during maturation in new oak barrels for up to 60 months in order to establish the relationship between the age of the distillate and the content of phenolic compounds extracted from the wood. The evaluation was based on the analyses of liginin derived compounds using high‐performance liquid chromatography. The level of maturation of aged cachaça can be characterised by evaluating the low molecular weight lignin‐derived phenolic substances. The total amount of benzoic acids (vanillic and syringic acids) can be taken into consideration for predicting the level of maturation of distillates. Based on the composition of maturation related congeners, it is likely that for cachaça, each year of aging in new oak barrels corresponds to approximately five years of aging for spirits in general. © 2020 The Institute of Brewing & Distilling     

Ethyl carbamate in the production and aging of cachaça in oak (Quercus sp.) and amburana (Amburana cearensis) barrels

There are residual organic and inorganic contaminants in the cachaça production chain. Among the organic contaminants, ethyl carbamate has been widely studied. It is formed naturally during the fermentation processes and can be found in many foods and beverages such as bread, yoghurt, wine, beer and especially in fermented–distilled beverages such as whiskey, rum, vodka, grappa, cachaça and tiquira. The objective of this study was to identify and quantify ethyl carbamate during the steps of the production process and aging of cachaça in oak (Quercus sp) and amburana (Amburana cearensis) barrels. The cane used for cachaça production, as well as the process for obtaining the fermentation broth, did not affect the formation of ethyl carbamate, as it was not detected. Carbamate was detected in low concentrations, but was not quantified, in the fermentation, distillation and aging steps. Copyright © 2014 The Institute of Brewing & Distilling     

Physicochemical profile and determination of volatile compounds in cachaça stored in new oak (Quercus sp.), amburana (Amburana cearensis), jatoba (Hymenaeae carbouril), balsam (Myroxylon peruiferum) and peroba (Paratecoma peroba) casks by SPME‐GC–MS

Aging has become common practice among producers seeking to increase the value of their products. The objective of this work was to conduct periodic monitoring by solid‐phase microextraction–gas chromatography–mass spectrometry of the physical and chemical quality of aging cachaça in terms of the alcohol content, volatile acidity, esters, aldehydes, higher alcohols, furfural, methanol, dry extract, copper and volatile compounds in the production process (distilled fractions) and during storage in casks newly made from oak (Quercus sp.), amburana (Amburana cearensis), jatoba (Hymenaeae carbouril), balsam (Myroxylon peruiferum) and peroba (Paratecoma peroba). The barrels were made in a specialized cooperage, and cachaça was obtained from a production unit in the southern region of Minas Gerais. Distinct physicochemical values were obtained for the distilled fractions; head and tail fractions had inappropriate concentrations of alcohol, aldehydes and butan‐1‐ol. Values within the limits established by law were obtained for the heart fraction, both in the distillation process and during aging, and it is, therefore, suitable for consumption. Several important compounds responsible for the aroma and flavour of the cachaças were observed, and alcohols, acids, esters and sesquiterpenes were found to compose the main groups. Through variance and main component analysis, important chemical changes were observed in the beverages. Copyright © 2016 The Institute of Brewing & Distilling     

Aging marker profile in cachaça is influenced by toasted oak chips

Cachaça is the most important distilled spirit in Brazil and the fourth most consumed in the world. Aging is not mandatory for cachaça. When aging is carried out, casks generally do not undergo the final wood toasting. However the level of thermal degradation of wood influences the formation of new chemical compounds, which are released during the aging process and improve the quality of the spirit. The objective of this study was to verify the influence of origin of wood and toasting intensity of oak chips on the profile of aging markers in cachaça. Staves of oak wood from the forests of Allier, Vosges and Nièvre (France) were milled and screened at 9 mesh. The chips underwent light, medium and heavy toasting. The toasted chips were added to cachaça (1 g/L) and kept in a closed system at room temperature, without agitation, for 15 days. The aging congeners (gallic acid, 5‐hydroxymethylfurfural, furfural, vanillin, vanillic acid, syringaldehyde, sinapaldehyde, syringic acid and coniferaldehyde) were analysed using HPLC. The increase in toasting intensity enhanced the content of the aging markers in cachaça, especially syringic acid, vanillin, syringaldehyde, coniferaldehyde and sinapaldehyde. The generation of aging marker compounds was influenced only by the toasting intensity and not by the origin of the oak wood. Copyright © 2015 The Institute of Brewing & Distilling     

Effect of co-inoculation of Saccharomyces cerevisiae and Lactobacillus fermentum on the quality of the distilled sugar cane beverage cachaça

Abstract: The effect of Lactobacillus fermentum in co‐inoculation with Saccharomyces cerevisiae UFLA CA11 on the quality of cachaça (sugar cane spirit) was evaluated. The co‐inoculation was first evaluated in flask fermentation, and subsequently, yeast and bacteria were co‐cultured at approximately 10⁵ CFU/mL and 10⁸ CFU/mL, respectively, in 4 consecutive batches. L. fermentum did not affect the growth or activity (sugar consumption and fermentation rate) of S. cerevisiae UFLA CA11 during fermentation. The physicochemical analysis revealed a higher concentration (Tukey test) of aldehydes (22.07 mg/100 mL anhydrous alcohol) in cachaça produced by co‐inoculation. Analysis of volatile compounds using GC‐FID demonstrated that cachaça produced by co‐inoculation had higher concentrations of acetaldehyde (25.15 mg/L), ethyl acetate (30.17 mg/L), and 2,3‐butanedione (170.39 μ/L), while cachaça produced by UFLA CA11 contained higher concentrations of ethyl lactate (1205.98 μ/L), propionic acid (127.97 μ/L), butyric acid (2335.57 μ/L), and 1‐pentanol (469.23 μ/L). The lowest concentration of acetic acid measured by HPLC was found in cachaça obtained with UFLA CA11. The sensory analysis, performed using the Mann–Whitney test, revealed that cachaça produced by co‐inoculation differed from that produced by UFLA CA11 in taste and aroma. Practical Application: This study reports on the use of a mixed culture of Saccharomyces cerevisae and Lactobacillus fermentum to produce cachaça and shows the influence of co‐inoculation of yeast and bacteria on the quality of this beverage.     

Cachaça stored in casks newly constructed of oak (Quercus sp.), amburana (Amburana cearensis), jatoba (Hymenaeae carbouril), balsam (Myroxylon peruiferum) and peroba (Paratecoma peroba): alcohol content,phenol composition,colour intensity and dry extract

Aging is the last stage of the cachaça production process. The containers used for aging are wooden barrels and casks, which act as a semi‐permeable membrane, allowing the passage of alcohol and water vapours. This passage is a function of the relative humidity and the temperature of the storage location. The wood traditionally used in Brazil is oak. However, various native woods of Brazilian origin have been used in the manufacture of barrels. The principal compounds extracted from wood by the distillates are volatile compounds, phenolic compounds, tannic substances, sugars, glycerol and non‐volatile organic acids. The objectives of this study were to evaluate and compare the phenolic substances found in cachaça stored in recently constructed oak, amburana, Jatoba, balsam and peroba casks. We evaluated some physicochemical parameters that changed during the storage process. After 12 months of storage, we observed a decrease in alcohol content and an increase in dry extract. An increase in total phenolic compounds and colour intensity was observed, and there was a strong linear correlation between total phenolic compounds, solids and colour intensity. According to the results for the phenols analysed by HPLC, a progressive increase in all the compounds and a heterogeneity in all woods used for the storage of beverages were observed. Copyright © 2017 The Institute of Brewing & Distilling     

Fatty acid composition and sensory properties of Wels catfish (Silurus glanis) hot smoked with different sawdust materials

This study aims to compare chemical, physical and sensorial parameters of the Wels catfish (Silurus glanis), hot smoked using vine, poplar, lemon tree and oak sawdust as well as corncob. Significant differences (P < 0.05) in proximate composition were found between fresh and smoked samples; however, the changes in fatty acid composition were less significant. In the fatty acid composition of control group, monounsaturated fatty acids (41.60%) had the highest share in fatty acids, which was followed by saturated fatty acids (29.95%) and polyunsaturated fatty acids (28.34%). The major fatty acids were observed to be C16:0, C18:0; C16:1 n‐7, C18:1 n‐9c, C18:1 n‐9t and C18:2 n6c. There were significant differences (P < 0.05) between the groups considering their colour measurement results. General preference criteria such as appearance, odour, texture, colour and taste were chosen for the sensorial analysis, which were rated by the panellists. According to the results of overall appearance, the fillet pieces smoked with lemon tree (9.00), poplar (8.66), corncob (8.00), oak (7.33) and vine (5.33) sawdust were determined as the most preferred, in order.     

Chemical Typification of the Sugarcane Spirits Produced in São Paulo State

To typify São Paulo State sugarcane spirits, 37 chemical compounds were analyzed in 81 Brazilian sugarcane spirits (cachaça), which were produced in different cities from São Paulo State. Among these samples, 56 were distilled in copper alembics, and the other 25 were distilled in steel columns. Hierarchical cluster analysis and principal component analysis were performed with both chemical data sets. The chemical profiles of the cachaças distilled in the column apparatus formed 4 specific clusters, which correspond to 4 distinct geographic regions of São Paulo State. For the cachaças that were distilled in copper alembics, 2 cachaça clusters were formed; however, no correlation between their respective chemical similarities and geographical origins was observed.     

Influence of wood origin in the polyphenolic composition of a Spanish red wine aging in bottle, after storage in barrels of Spanish, French and American oak wood

In this paper, the changes in the composition of a red wine obtained from Tempranillo grapes (Vitis vinifera L.), stored from 12 to 24 months in bottles were studied. The wine was previously aging for 21 months in barrels made of Spanish oak wood (Quercus spp.). The changes of chromatic data, global polyphenolic families assessment (polyphenols, catechins, proanthocyanidins and anthocyanins) and individually polyphenols by HPLC during their storage time in bottles were studied and compared with these of the same wine aged in barrels made of French oak and American oak and stored in bottle for 24 months. Samples of wines obtained after 12 months in bottle were also compared with those after 24 months. The stepwise discriminant analysis with data of chromatic parameters and global polyphenolic families indicates that the wines aged in Spanish and French oak wood barrels, after 24 months stored in bottle, have similar characteristics, but they are significantly different to those of wines aged in barrels made of American oak wood. Regarding the analysis of individually non-anthocyanic polyphenols, discriminant analysis shows that wines stored for 24 months in bottle, aged in barrels made of Spanish, French and American oak woods, show overlapping results, while those from wines after 12 months in bottle are more dispersed. The discriminant analysis carried out on anthocyanidin concentrations of wines stored 24 months in bottles has shown three groups according the kind of wood used, indicating that wines aged in Spanish and French oak barrels are much more similar in anthocyanidin concentrations than those aged in the American barrels.     

Concentration of volatile compounds in Chardonnay wine fermented in stainless steel tanks and oak barrels

The influence of the type of container used in alcoholic fermentation on the formation of volatile compounds in wine from Chardonnay variety was studied. To do so, must from Chardonnay variety was fermented in both stainless steel tanks and in new Nevers oak barrels. The results obtained showed that wine fermented in barrels had a greater concentration of higher alcohols and esters than wine fermented in tanks. Concentration of isoamyl acetate, ethyl hexanoate, ethyl octanoate and ethyl decanoate was four times higher in wine fermented in oak barrels than in wine fermented in stainless steel tanks. With regard to the concentration of acids, a greater concentration of medium-chain fatty acids (C6:0–C10:0) was noticeable in wine fermented in oak barrels. Given that these acids are toxic for the yeasts, they may be responsible for the slower fermentation rate of wine fermented in oak barrels.     

Use of microfungi in the treatment of oak chips: possible effects on wine

BACKGROUND: Oak barrels are commonly used in the aging of wines and spirits because of their positive effects on the product. In recent years the addition of oak chips has been used to introduce desirable wood aromas and flavours into wines. In this study, oak chips in saline solution or laboratory medium were inoculated with Penicillium purpurogenum, Aureobasidium pullulans, Phialemonium obovatum, Phanerochaete chrysosporium and a combination of Ph. chrysosporium and A. pullulans. After 12 weeks of incubation, oak chips (2 g L^?1) were macerated in a red wine for 17 days. Gas chromatography/mass spectrometry and high‐performance liquid chromatography were used to evaluate 14 compounds, namely furfural, furfuryl alcohol, guaiacol, syringol, cis‐β‐methyl‐γ‐octalactone, 2‐phenylethanol, 4‐vinylguaiacol, benzyl alcohol, 2,3‐butanediol, γ‐butyrolactone, benzaldehyde, 4‐ethylguaiacol, gallic acid and ellagic acid. RESULTS: The microfungal treatments increased the concentration of some components. In particular, P. purpurogenum resulted in a significant improvement in the levels of guaiacol, furfural, syringol, furfuryl alcohol and 2‐phenylethanol. CONCLUSION: Penicillium purpurogenum and Ph. chrysosporium showed a constant trend (enrichment of furfural and benzaldehyde) independent to some extent of the medium used for chip treatment. Copyright © 2010 Society of Chemical Industry     

Effect of light on the concentration of ethyl carbamate in cachaça stored in glass bottles

This study sought to evaluate the influence of natural light on the concentration of ethyl carbamate (EC) in cachaças aged in wooden barrels and stored in glass bottles for a period of 6 months. The quantification of EC was achieved by HPLC using a fluorescence detector after previous derivation of the samples and standards with 9‐xanthydrol. All of the samples presented an EC concentration below the limit established by Brazilian legislation. The highest concentration found was 79.70 µg L^?1. As for the influence of light and storage period, 70% of the samples exhibited an influence of these parameters. Copyright © 2015 The Institute of Brewing & Distilling     

Comparison of Transesterification Methods for Fatty Acid Analysis in Higher Fungi: Application to Mushrooms

This study evaluated the effectiveness of two commonly used transesterification methods for the preparation of fatty acid methyl esters (FAMEs) for gas chromatographic analysis. A combination of base followed by acid catalysis [potassium hydroxide/sulfuric acid/methanol (KOH–H₂SO₄–MeOH)] was compared to an acid-only catalyst [methanolic–boron trifluoride (BF₃–MeOH)] for the quantification of the fatty acid content in mushrooms after preextraction of total lipids with chloroform/methanol (2:1 v/v). The mushrooms studied were commonly cultivated species, Agaricus bisporus (brown) and A. bisporus (white), and three wild medicinal mushrooms, turkey tail (Trametes versicolor), artist conk (Ganoderma applanatum), and tinder polypore (Fomes fomentarius). The major fatty acids identified were palmitic (C16:0), stearic (C18:0), oleic (C18:1), and linoleic acid (18:2n6) which constituted 80% to 90% of the total amount. Variation due to the FAME preparation methods was observed in both minor and major fatty acids. Another major observation made between the two methods was the total number of individual fatty acids (FAs) methylated. The base and acid transesterification procedure resulted in the identification of 42 FAMEs, whereas with the acid 38 FAMEs were observed. Therefore, the research recommends the use of a base–acid combination for preparation of FAMEs in mushroom lipids.     

Identification of substances responsible for the ‘sawdust’ aroma in oak wood

The unpleasant ‘sawdust’ odour sometimes found in wines aged in new barrels was studied by gas chromatography olfactory detection and mass spectrometry. A particular aromatic zone has several chromatographic peaks, corresponding to certain characteristic odours which can be detected by smelling the gas effluent. These include the subtle rancid, weedy odour of ‘sawdust’. Various carbonyl components have been identified in this particular zone. These include (E)-2-nonenal, 3-octen-1-one, (E)-2-octenal and 1-decanal. These molecules are the primary cause of disagreeable oak wood odours. By measuring (E)-2-nonenal in wines, after derivation by O-(2,3,4,5-pentafluobenzyl)-hydroxilamine (PFBOA), it was possible to correlate the concentration of this unsaturated aldehyde with the intensity of the ‘sawdust’ character noted in tasting. The possible explanations for the presence of these carbonyl compounds are debatable. The carbonyl content varied from one wood sample to another. However, controling the toasting of the wood, both in the laboratory and in the cooperage, produced a major reduction in the extractable (E)-2-nonenal content and eradicated the ‘sawdust’ character of the wine. © 1998 SCI.     

Impact of wood species on microbial community composition,beer chemistry and sensory characteristics during barrel-ageing of beer

Barrel-ageing of conventionally fermented beers is becoming increasingly popular in recent years, but only very little is known about the underlying process. In this study, we show that wood species significantly affects the bacterial community composition, beer chemistry and sensory characteristics throughout 38 weeks of barrel-ageing. Whereas the microbial communities of oak- and acacia-aged beer became dominated by Pediococcus damnosus and Brettanomyces bruxellensis, beer aged in oak barrels also contained a large fraction of Acetobacter sp. (29.34%) and to a lesser extent Paenibacillus sp. (2.74%) that were almost undetected in acacia-aged beer. Oak barrels also imparted substantial concentrations of eugenol, lactones and vanillin, while acacia-aged beer contained high concentrations of total polyphenols and β-glucan, which also translated into different sensory perceptions. Altogether, our results provide novel insights into the barrel-ageing process of beer, and may pave the way for a new generation of beers with a noteworthy flavour complexity.     

Use of acacia barrique barrels – Influence on the quality of Malvazija from Istria wines

In order to improve Malvazija from Istria wine quality, we used two types of barrels: oak (of French and Croatian origin) and acacia (of Croatian origin). After 12 months ageing period all of the wines were analysed chemically and sensorially. Results showed marked differences between oak and acacia aged wines, especially in simple volatile phenol and oak lactones concentrations. During the ageing period a significant increase in furfural, 5-methylfurfural, guaiacol, eugenol and trans-eugenol was noticed. Results pointed out the importance of choosing the right barrels (oak or acacia) and time of leaving the wine in the barrels to achieve the desired goal. The highest rated wines were made in acacia barrels.