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Thesis (M.Sc. (Hons.)) -- University of Western Sydney, 2001. / "A thesis submitted in partial fulfilment of the requirements for the degree of Master of Science (Honours), University of Western Sydney, Hawkesbury" Bibliography : leaves 60-66.

Características sensoriais diferenciadas e qualidade química podem garantir a competitividade de uma bebida destilada. O uísque é uma bebida alcoólica produzida a partir da destilação do mosto fermentado de cereais e que passa por um período de maturação em barris de carvalho. A cachaça, por sua vez, é produzida a partir da destilação do caldo de cana-de-açúcar fermentado. O objetivo deste trabalho foi analisar a qualidade química e sensorial da bebida destilada oriunda das matérias-primas cana-de-açúcar e cevada e produzida mediante técnicas já existentes em processos produtivos de cachaça e uísque. O mosto combinado teve como fonte de açúcares o mosto de caldo de cana e o mosto de malte de cevada, que foram preparados separadamente e depois misturados nas seguintes proporções em porcentagem: 100 (A), 75 (B), 50 (C), 25 (D) e 0 (E) de caldo de cana, complementado com o mosto de malte de cevada. O processo fermentativo foi conduzido a 30ºC, mediante adição de leveduras Saccharomyces cerevisiae, cepas CA-11 e S-33, inoculando-se 1,5 g/L de cada levedura. As destilações foram realizadas em alambique de cobre, seguindo a metodologia de dupla-destilação utilizada para a produção de Scotch malt whisky. As bebidas duplamente destiladas foram acondicionadas em barris de carvalho por 60 dias. Os mostos foram submetidos às análises de pH, Brix, Pol, Açúcares Redutores (AR), Açúcares Redutores Totais (ART) e Acidez Total; e os vinhos foram analisados quanto a Teor Alcoólico, pH, Açúcares Redutores Residuais (ARR) e Acidez Total. Os flegmas, bidestilados e as bebidas envelhecidas foram submetidos a análises de teor alcoólico (densitometria), cobre (colorimetria), congêneres voláteis (CG-FID) e carbamato de etila (CG-EM). As bebidas envelhecidas também foram submetidas a análises de intensidade de cor e compostos fenólicos totais (espectrofotometria) e congêneres de maturação (CLAE). Testes sensoriais foram realizados para verificar a preferência entre as amostras pelos consumidores. Análises estatísticas foram realizadas pelo programa SAS (ANOVA e Testes de Tukey). Foi comprovada a eficiência da técnica de bidestilação na redução de alguns compostos limitados pela legislação. Mostos combinados com maior porcentagem de malte de cevada apresentaram menor formação de carbamato de etila. O envelhecimento aumentou a concentração de carbamato de etila nos destilados A, B e C sendo ao final o único contaminante presente acima dos limites permitidos pela legislação de aguardente de cana. Siringaldeído e ácido gálico foram os congêneres de maturação com as maiores concentrações nos destilados. O destilado do tratamento A apresentou a maior concentração total de compostos de envelhecimento. Na análise sensorial o destilado do tratamento C apresentou a maior preferência pelos provadores. Este estudo comprova que a produção de uma nova bebida a partir da combinação de matérias-primas diferentes pode apresentar resultados satisfatórios. Entretanto, ressalta-se a importância da continuidade desse estudo para afinar a definição da combinação de mostos mais adequada, para assim confirmar a viabilidade e eficiência do processo. / Differentiated sensory characteristics and chemical quality can ensure the competitiveness of a distilled beverage. Whisky is an alcoholic beverage produced from the distillation of fermented worts of cereals and aged in oak barrels. Cachaça, in turn, is produced from the distillation of fermented sugarcane juice. The objective of this study was to analyze the chemical and sensory quality of distilled spirit derived sugarcane and barley and produced by existing techniques in production processes of cachaça and whisky. The combined wort had as a source of sugars the sugarcane juice and barley malt wort, that were prepared separately and then mixed in the following proportions by percentage: 100 (A) 75 (B), 50 (C), 25 (D) and 0 (E) of sugarcane juice, supplemented with barley malt wort. The fermentation was conducted at 30° C by addition of Saccharomyces cerevisiae, CA-11 and S-33 strains, inoculating 1,5 g/L of each yeast. The distillations were performed in copper still, according to double-distillation method used for production of Scotch malt whisky. Double-distilled spirits were stored in oak barrels for 60 days. Worts were submitted to analysis of pH, Brix, Pol, Reducing Sugars (AR), Total Reducing Sugars (ART) and Total Acidity; and the wines were analyzed for Alcohol, pH, Residual Reducing Sugars (ARR) and Total Acidity. Low wines, double-distilled spirits and aged spirits were analyzed for alcohol content (densitometry), copper (colorimetry), volatile congeners (GC-FID) and ethyl carbamate (GC-MS). Aged spirits were also analyzed for color intensity and total phenolic compounds (spectrophotometry) and aged congeners (HPLC). Sensory tests were conducted to verify preference between samples by consumers. Statistical analyzes were performed using SAS (ANOVA and Tukey tests). The efficiency of double-distillation technique in reduce some compounds limited by legislation was confirmed. Worts combined with a higher percentage of barley malt showed lower formation of ethyl carbamate. Aging increased the concentration of ethyl carbamate in spirits A, B and C being at the end the only contaminant found above the limits allowed by the cachaça legislation. Syringaldehyde and gallic acid were the aged congeners with the highest concentrations in the spirits. Spirit A had the highest total concentration of aged congeners. Sensory analysis showed that spirit C was the most preferred by tasters. This study demonstrates that the production of a new beverage from the combination of different raw materials can provide satisfactory results. However, it emphasizes the importance of continuing this study to refine the definition of the most appropriate combination of worts, thus to confirm the feasibility and process efficiency.

Características sensoriais diferenciadas e qualidade química podem garantir a competitividade de uma bebida destilada. O uísque é uma bebida alcoólica produzida a partir da destilação do mosto fermentado de cereais e que passa por um período de maturação em barris de carvalho. A cachaça, por sua vez, é produzida a partir da destilação do caldo de cana-de-açúcar fermentado. O objetivo deste trabalho foi analisar a qualidade química e sensorial da bebida destilada oriunda das matérias-primas cana-de-açúcar e cevada e produzida mediante técnicas já existentes em processos produtivos de cachaça e uísque. O mosto combinado teve como fonte de açúcares o mosto de caldo de cana e o mosto de malte de cevada, que foram preparados separadamente e depois misturados nas seguintes proporções em porcentagem: 100 (A), 75 (B), 50 (C), 25 (D) e 0 (E) de caldo de cana, complementado com o mosto de malte de cevada. O processo fermentativo foi conduzido a 30ºC, mediante adição de leveduras Saccharomyces cerevisiae, cepas CA-11 e S-33, inoculando-se 1,5 g/L de cada levedura. As destilações foram realizadas em alambique de cobre, seguindo a metodologia de dupla-destilação utilizada para a produção de Scotch malt whisky. As bebidas duplamente destiladas foram acondicionadas em barris de carvalho por 60 dias. Os mostos foram submetidos às análises de pH, Brix, Pol, Açúcares Redutores (AR), Açúcares Redutores Totais (ART) e Acidez Total; e os vinhos foram analisados quanto a Teor Alcoólico, pH, Açúcares Redutores Residuais (ARR) e Acidez Total. Os flegmas, bidestilados e as bebidas envelhecidas foram submetidos a análises de teor alcoólico (densitometria), cobre (colorimetria), congêneres voláteis (CG-FID) e carbamato de etila (CG-EM). As bebidas envelhecidas também foram submetidas a análises de intensidade de cor e compostos fenólicos totais (espectrofotometria) e congêneres de maturação (CLAE). Testes sensoriais foram realizados para verificar a preferência entre as amostras pelos consumidores. Análises estatísticas foram realizadas pelo programa SAS (ANOVA e Testes de Tukey). Foi comprovada a eficiência da técnica de bidestilação na redução de alguns compostos limitados pela legislação. Mostos combinados com maior porcentagem de malte de cevada apresentaram menor formação de carbamato de etila. O envelhecimento aumentou a concentração de carbamato de etila nos destilados A, B e C sendo ao final o único contaminante presente acima dos limites permitidos pela legislação de aguardente de cana. Siringaldeído e ácido gálico foram os congêneres de maturação com as maiores concentrações nos destilados. O destilado do tratamento A apresentou a maior concentração total de compostos de envelhecimento. Na análise sensorial o destilado do tratamento C apresentou a maior preferência pelos provadores. Este estudo comprova que a produção de uma nova bebida a partir da combinação de matérias-primas diferentes pode apresentar resultados satisfatórios. Entretanto, ressalta-se a importância da continuidade desse estudo para afinar a definição da combinação de mostos mais adequada, para assim confirmar a viabilidade e eficiência do processo. / Differentiated sensory characteristics and chemical quality can ensure the competitiveness of a distilled beverage. Whisky is an alcoholic beverage produced from the distillation of fermented worts of cereals and aged in oak barrels. Cachaça, in turn, is produced from the distillation of fermented sugarcane juice. The objective of this study was to analyze the chemical and sensory quality of distilled spirit derived sugarcane and barley and produced by existing techniques in production processes of cachaça and whisky. The combined wort had as a source of sugars the sugarcane juice and barley malt wort, that were prepared separately and then mixed in the following proportions by percentage: 100 (A) 75 (B), 50 (C), 25 (D) and 0 (E) of sugarcane juice, supplemented with barley malt wort. The fermentation was conducted at 30° C by addition of Saccharomyces cerevisiae, CA-11 and S-33 strains, inoculating 1,5 g/L of each yeast. The distillations were performed in copper still, according to double-distillation method used for production of Scotch malt whisky. Double-distilled spirits were stored in oak barrels for 60 days. Worts were submitted to analysis of pH, Brix, Pol, Reducing Sugars (AR), Total Reducing Sugars (ART) and Total Acidity; and the wines were analyzed for Alcohol, pH, Residual Reducing Sugars (ARR) and Total Acidity. Low wines, double-distilled spirits and aged spirits were analyzed for alcohol content (densitometry), copper (colorimetry), volatile congeners (GC-FID) and ethyl carbamate (GC-MS). Aged spirits were also analyzed for color intensity and total phenolic compounds (spectrophotometry) and aged congeners (HPLC). Sensory tests were conducted to verify preference between samples by consumers. Statistical analyzes were performed using SAS (ANOVA and Tukey tests). The efficiency of double-distillation technique in reduce some compounds limited by legislation was confirmed. Worts combined with a higher percentage of barley malt showed lower formation of ethyl carbamate. Aging increased the concentration of ethyl carbamate in spirits A, B and C being at the end the only contaminant found above the limits allowed by the cachaça legislation. Syringaldehyde and gallic acid were the aged congeners with the highest concentrations in the spirits. Spirit A had the highest total concentration of aged congeners. Sensory analysis showed that spirit C was the most preferred by tasters. This study demonstrates that the production of a new beverage from the combination of different raw materials can provide satisfactory results. However, it emphasizes the importance of continuing this study to refine the definition of the most appropriate combination of worts, thus to confirm the feasibility and process efficiency.

<p>Cilj istraživanja doktorske disertacije je bio da se u<br />konitnuitetu ispita sadržaj ukupnih fenola, fenolnih kiselina i<br />anitoksidativna aktivnost (antiradikalska aktivnost na DPPH i<br />hidroksil radikale) u toku proizvodnje slada i piva (u ječmu,<br />namočenom ječmu, zelenom sladu, sladu, sladovini, ohmeljenoj<br />sladovini, sladovini tokom fermentacija, mladom pivu i pivu)<br />proizvedenih od tri priznate sorte pivskog ječma: NS 525, NS<br />565 i NS 583.<br />Sadržaj ukupnih fenola u uzorcima ječma je bio: NS 525 -<br />0,76; NS 565 - 0,75 i NS 583 - 0,70 mg GAE/g suve materije.<br />Sadržaj ukupnih fenola u svim proizvednim sladovima (0,96;<br />0,94 i 0,91 mg GAE/g suve materije za NS 525; NS 565 i NS<br />583) je bio vi&scaron;i od sadržaja u ječmu. Sorta NS 525 je imala<br />najvi&scaron;i sadržaj ukupnih fenola tokom svih faza sladovanja, dok<br />su sorte NS 565 i NS 583 imale niže sadržaje ukupnih fenola.<br />Najniži sadržaj ukupnih fenola imala je sorta NS 583.<br />U svim ispitivanim sortama ječma ferulna, p-kumarinska i<br />vanilinska kiselina su bile dominantne u uzorcima ječma,<br />tokom sladovanja i u proizvedenom sladu.<br />Sadržaj ukupnih fenolnih kiselina u ječmu je iznosio za sortu<br />NS 525 - 200,98; NS 565 - 184,10 i za NS 583 &ndash; 177,27 &mu;g/g suve<br />materije. Sadržaj ukupnih fenolnih kiselina je rastao kod svih<br />ispitivanih sorti tokom močenja i dostigao maksimum u toku<br />prvog dana klijanja za NS 525 &ndash; 548,31; NS 565 &ndash; 518,65 i NS<br />583 &ndash; 517,17 &mu;g/g suve materije. Dobijeni rezultati su pokazali<br />da je proces sladovanja imao značajan uticaj na sadržaj<br />pojedinačnih i ukupnih fenolnih kiselina.<br />Sorta NS 525 je imala najvi&scaron;u antiradikalsku aktivnost na<br />DPPH radikale (EC50 za NS 525 - 0,658; NS 565 - 0,667 i NS<br />583 - 0,758 mg/ml) &scaron;to pokazuje da sorta ječma ima uticaja na<br />antiradikalsku aktivnost na DPPH radikale. Za ispitivane sorte<br />ječma, antiradikalska aktivnost na DPPH radikale se povisila<br />značajno tokom močenja. U proizvedenim sladovima<br />antiradikalska aktivnost na DPPH radikale bila je vi&scaron;a nego u<br />ječmu. Trend porasta i smanjenja antiradikalske aktivnosti na<br />DPPH radikale tokom sladovanja je bio isti za sve ispitivane<br />sorte ječma.<br />Antiradikalska aktivnost na hidroksil radikale, izražena kao<br />EC50 vrednost, u ispitivanim sortama ječma je iznosila: NS 525<br />&ndash; 0,352; NS 565 &ndash; 0,385 i NS 583 &ndash; 0,455 mg/ml. Može se<br />zaključiti da je sorta NS 525 imala najvi&scaron;u antiradikalsku<br />aktivnost na hidroksil radikale. Antiradikalska aktivnost na<br />hidroksil radikale se znatno povisila tokom močenja. U<br />proizvedenom sladu je antiradikalska aktivnost na hidroksil<br />radikale bila vi&scaron;a nego u ječmu. Trend porasta i smanjenja<br />antiradikalske aktivnosti na hidroksil radikale tokom<br />sladovanja je bio isti za sve ispitivane sorte ječma.<br />Sorta NS 525 je imala najvi&scaron;i sadržaj ukupnih fenola kao i<br />najvi&scaron;u antioksidativnu aktivnost tj. DPPH i hidroksil<br />antiradikalsku aktivnost. Ovi rezultati pokazuju da sorta<br />ječma može da utiče na antiradikalske osobine slada. Sorta NS<br />525 je imala najvi&scaron;i sadržaj ukupnih fenola, ukupnih fenolnih<br />kiselina i najvi&scaron;u antiradikalsku aktivnost na DPPH i hidroksil<br />radikale u toku sladovanja.<br />U svim proizvedenim sladovinama, ohmeljenim sladovinama i<br />pivima, ferulna, p-kumarinska, vanilinska i sinapinska kiselina<br />su imale najvi&scaron;e sadržaje. Sadržaj svih ispitivanih fenolnih<br />kiselina je povi&scaron;en nakon hmeljenja. Najvi&scaron;i ukupni sadržaj<br />fenolnih kiselina je odre&ntilde;en u ohmeljenim sladovinama (NS<br />525 - 461,41, NS 565 - 426,22 i NS 583 - 423,56 &mu;g/100ml).<br />Sadržaj ukupnih fenolnih kiselina je u svim proizvedenim<br />pivima bio niži u odnosu na odgovarajuće ohmeljene sladovine.<br />U sladovini proizvedenoj iz slada NS 525 je odre&ntilde;ena najvi&scaron;a<br />antiradikalska aktivnost na DPPH i hidroksil radikale &scaron;to<br />ukazuje da antiradikalska aktivnosti komponenti slada ima<br />uticaja na antiradikalsku aktivnost proizvedene sladovine. U<br />ispitivanim sladovinama, nakon hmeljenja se znatno povisila<br />antiradikalska aktivnost na DPPH i hidroksil radikale.<br />Antiradikalska aktivnost na DPPH i hidroksil radikale se<br />smanjila tokom glavne i naknadne fermentacije.<br />U sladovini proizvedenoj od slada NS 525 sa najvi&scaron;im<br />sadržajem ukupnih fenola i ukupnih fenolnih kiselina<br />odre&ntilde;ena je najvi&scaron;a antiradikalska aktivnost na DPPH i<br />hidroksil radikale. Tokom proizvodnje piva sadržaj ukupnih<br />fenola se blago smanjio, &scaron;to ukazuje da je proces proizvodnje<br />imao uticaja na njihov sadržaj. Trend smanjenja<br />antiradikalske aktivnosti na DPPH i hidroksil radikale<br />odgovara smanjenju sadržaja ukupnih fenola i ukupnih<br />fenolnih kiselina tokom procesa proizvodnje piva.<br />Primenjena GC-MS metoda za odre&ntilde;ivanje sadržaja fenolnih<br />kiselina tokom procesa proizvodnje slada i piva se pokazala<br />kao osetljiva, specifična i dobre ponovljivosti. Može se<br />primeniti za odre&ntilde;ivanje sadržaja fenolnih kiselina u ječmu,<br />namočenom ječmu, zelenom sladu, sladu, sladovini, ohmeljenoj<br />sladovini, tokom fermentacije i u pivu.<br />Sadržaj ukupnih fenola, fenolnih kiselina i antioksidativna<br />aktivnost slada, koji se koristi za proizvodnju piva, imaju<br />značajan uticaj na antioksidativnu aktivnost piva.<br />Razumevanje promena sadržaja fenolnih kiselina i<br />antioksidativne aktivnosti tokom proizvodnje slada i piva može<br />nam pružiti vredne informacije o za&scaron;titi endogenih<br />antioksidanata u proizvodnji piva. Na taj način mogu se<br />proizvoditi piva sa vi&scaron;om antioksidativnom aktivno&scaron;ću i prema<br />tome i povi&scaron;enom otporno&scaron;ću prema lipidnoj oksidaciji i<br />starenju piva.</p> / <p>Studies carried out in the frame of the doctorial thesis<br />aimed at continuous determination of the content of<br />total phenolics, phenolic acids and antioxidant activity<br />(antiradical activity on DPPH and hydroxyl radicals)<br />during malt and beer production (in barley, steeped<br />barley, green malt, malt, wort, hopped wort,<br />fermenting wort, green beer, and beer) produced from<br />three accepted brewer&rsquo;s barley varieties: NS 525, NS<br />565, and NS 583.<br />The total phenolics content in the barley samples was<br />0.76 for NS 525, 0.75 for NS 565 and 0.70 mg GAE/g<br />dry matter (d.m.) for NS 583. Higher content of total<br />phenolics was determined in the malt samples in<br />comparison with the barley samples: (0.96, 0.94, and<br />0.91 mg GAE/g d.m. for NS 525, NS 565, and NS 583,<br />respectively). Variety NS 525 was the highest in total<br />phenolics content during all stages of malting when<br />compared to the other varieties. The lowest content of<br />total phenolics was found in the variety NS 583.<br />In all examined samples, ferulic, p-coumaric and<br />vanillic acid dominated in the barley samples, during<br />malting and in the produced malts.<br />Content of total phenolic acids in the barley samples<br />was 200.98 for NS 525, 184.10 for NS 565 and 177.27<br />mg/g d.m. for NS 583. During steeping, the content of<br />total phenolic acids increased for all samples reaching<br />the maximum at the first day of germination (NS 525 &ndash;<br />548.31; NS 565 &ndash; 518.65, and NS 583 &ndash; 517.17 &mu;g/g<br />d.m.). The obtained results revealed that the malting<br />process had significant impact on the content of total<br />and individual phenolic acids.<br />Variety NS 525 showed the highest antiradical activity<br />on DPPH radicals (EC50 for NS 525 was 0.658, for NS<br />565 0.667, and for NS 583 0.758 mg/ml) indicating that<br />barley variety influences the antiradical activity on<br />DPPH radicals. Antiradical activity on DPPH radicals<br />significantly increased during steeping for all<br />investigated barley varieties. Higher antiradical<br />activity on DPPH radicals was determined in<br />produced malts when compared to corresponding<br />barley varieties. Similar increasing and decreasing<br />trends in the antiradical activity on DPPH radicals<br />during malting were observed in all investigated<br />barley varieties.<br />The antiradical activity on hydroxyl radicals,<br />expressed as EC50 value, in investigated barley<br />varieties, was: 0.325 for NS 525, 0.385 for NS 565, and<br />0.455 mg/ml for NS 583. It can be concluded that<br />barley variety NS 525 showed the highest antiradical<br />activity on hydroxyl radicals. The antiradical activity<br />on hydroxyl radicals significantly increased during<br />steeping. Higher antiradical activity on hydroxyl<br />radicals was determined in produced malts when<br />compared to corresponding barley varieties. Similar<br />increasing and decreasing trends in the antiradical<br />activity on hydroxyl radicals during malting were<br />observed in all investigated samples.<br />Variety NS 525 had the highest content of total<br />phenolics and exhibited the highest antioxidant<br />activity that is antiradical activity on DPPH and<br />hydroxyl radicals. These results suggest that variety<br />can influence the malt antiradical properties. Variety<br />NS 525 was the highest in total phenolics content, total<br />phenolic acids content and antiradical activity on<br />DPPH and hydroxyl radicals during malting.<br />The highest contents of ferulic, p-coumaric, vanillic,<br />and sinapic acids were determined in all wort, hopped<br />wort and beer samples. Increased contents of all<br />phenolic acids were observed after hopping. The<br />highest content of total phenolic acids was determined<br />in the hopped worts (461.41 for NS 525, 426.22 for NS<br />565, and 423.56 &mu;g/100 ml for NS 583. The beers<br />contained less total phenolic acids when compared to<br />the corresponding hopped worts.<br />Wort produced from NS 525 malt showed the highest<br />antiradical activity on DPPH and hydroxyl radicals<br />which indicates that the antiradical activity of malt<br />components affects the antiradical activity in produced<br />wort. After hopping, antiradical activity on DPPH and<br />hydroxyl radicals significantly increased in all worts.<br />The antiradical activity on DPPH and hydroxyl<br />radicals decreased during primary and secondary<br />fermentation.<br />Wort produced from NS 525 malt contained the<br />highest total phenolic content, total phenolic acids<br />content and showed the highest antiradical activity on<br />DPPH and hydroxyl radicals. During beer production,<br />content of total phenolic compounds slightly decreased<br />which indicates that production process had an<br />influence on their content. Similar decreasing trends<br />between the antiradical activity on DPPH and<br />hydroxyl radicals and the contents of total phenolics<br />and total phenolic acids during beer production were<br />observed.<br />The applied GC-MS method for determination of<br />phenolic acids contents during malt and beer<br />production was sensitive, specific and had good<br />repeatability. It can be used for determination of<br />phenolic acids content in barley, steeped barley, green<br />malt, malt, wort, hopped wort, during fermentation<br />and in beer.<br />The content of total phenolics, phenolic acids and<br />antioxidant activity of malt used for beer production<br />have significant influence on the beer antioxidant<br />activity. Understanding how the phenolic acids and<br />antioxidant activity change during malt and beer<br />production can provide valuable information about<br />the protection of endogenous antioxidants in beer<br />production. In this way, the production of beer with<br />enhanced antioxidant activity is possible and therefore<br />higher resistance to lipid oxidation and longer shelflife<br />could be introduced.</p>