Chemical composition of whiskies produced in ... - Dirk Lachenmeier

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148 Originalarbeiten « PC2 (4 %) PC2 (4%) 40 20 0 –20 –40 –60 0.8 0.6 0.4 0.2 0.0 Acetaldehyde W09 W07 n-propanol W08 W02, W06, W04, W03, W05 W01 –100 0 100 200 300 400 PC1 (95 %) Methanol Isobutanol Blended Scotch Single Malt Scotch Straight Bourbon Blended Bourbon Canadian Irish Brazilian 2-/3-methyl-1-butanol –0.2 0.0 0.2 0.4 0.6 0.8 1.0 PC1 (95%) Fig. 1 Explorative data analysis of the analytical results of 79 commercial whiskies. The Principal Component Analysis (PCA) shows both the scores (different whisky types, A) and loadings (names of analytes, B). Clear distinctions between BWB and SWB were observed. With the exception of the ratio of 2- + 3-methyl-1-butanol/isobutanol, average results of all major volatile congeners were considerably higher in SWB than in BWB, in particular n-propanol (+380 %), sum of n-propanol and 2- + 3-methyl-1-butanol (+235 %), isobutanol (+161%), total higher alcohols (+84 %), methanol (+107 %), and ethyl acetate (+77 %) (Tab. 1). These results are consistent with BWB being admixtures of malt whisky with highly rectified ethyl alcohol, probably fermented from sugar cane, which has considerably lower levels of higher alcohols and methanol when compared to grain or malt whisky [10]. With the exception of acetaldehyde, methanol, ethyl acetate, and higher alcohols (individually and combined) in the SWB brands (Tab. 1) fell within concentration ranges reported by Aylott and MacKenzie [10] previously for 20 brands of blended Scotch whisky bottled in Scotland (SWS). However, given the fact that acetaldehyde concentration in bottled whisky may change between 5 and 10 % [10], the differences in acetaldehyde levels between SWB and SWS are negligible. The result of the explorative data analysis of the GC quantitative results for 79 whiskies is shown in Figure 1. The PCA (A) (B) scores confirm that a considerable difference exists in the composition of the whiskies produced and bottled in different countries: Scotch, Irish, Canadian, Brazilian and Bourbon whisky groups are clearly seen. Two blended Scotch whiskies (W08 and W09) bottled in Brazil are in the Scotch group, whereas the other samples produced and bottled in Brazil (W01–W07) comprise a separate cluster on the score plot. Interestingly, multivariate statistics can also identify differences within one country group. Five Scotch samples with positive score values along PC1 are single malt, while the main group represent blended products. Straight bourbon whiskies (positive values of PC2) are also separated from blended products. The PCA loadings plot suggests that n-propanol and 2- and 3- methyl-1-butanol are characteristic compounds for Scotch and Bourbon brands. Conclusions This work has shown that all collected samples of blended whisky (produced and bottled in Brazil – BWB, and produced in Scotland and bottled in Brazil – SWB) comply with the Brazilian regulation for alcoholic strength, volatile acidity, acetaldehyde, methanol, ethyl acetate, higher alcohols (n-propanol, isobutanol and 2- + 3-methyl-1-butanol) and copper. Quantifiable level of ethyl carbamate was found in one brand of BWB only, at 0.09 mg/L. Results of major volatile congeners in SWB are consistent with blended whisky produced and bottled exclusively in Scotland. When compared to other countries, BWB showed much lower concentrations of methanol, ethyl acetate, n-propanol, and isobutanol. The use of highly rectified ethyl alcohol in the blending process is the most likely explanation for the lower levels of major volatile congeners in BWB. Acknowledgements ICCN and SPAO thank the Brazilian Government through CNPq [Projects 474644/2009-0 (edital 14/2009) and 552883/2010-7 (edital 70/2009)] for financial support. References [1] Laranjeira R et al.: Levantamento nacional sobre os padrões de consumo de álcool na população brasileira (in Portuguese). Brasília, Brazil: Secretaria Nacional Antidrogas. (Available from: bvsms.saude.gov.br/ bvs/publicacoes/relatorio_padroes_consumo_alcool.pdf) (2007). [2] Datamonitor: Industry profile. Spirits in Brazil. New York: Datamonitor. (Reference code, 0076-0801; Publication date, June 2011). [3] Whiskies: Whiskies mais vendidos no Brasil (in Portuguese). Whisky News, 2010, p. 139 (publication of the Sociedade Brasileira do Whisky, www.sbw.org.br). [4] Portaria: Portaria Nº 65 de 23 de abril de 2008 do Ministério da Agricultura, Pecuária e Abastecimento do Brasil. Diário Oficial da União, 78, Seção 1, p. 17 (2008). [5] Decreto: Decreto Nº 6.871 de 4 de junho de 2009 da Presidência da República do Brasil. Diário Oficial da União, 106, Seção 1, p. 26 (2009). [6] Regulation: Regulation (EC) No 110/2008 of the European Parliament and of the Council. Off J Eur Union L 39, 16–54 (2008). » 109. Jahrgang | März 2013 | DLR
[7] Instrução Normativa: Instrução Normativa Nº 13 de 29 de junho de 2005 do Ministério da Agricultura, Pecuária e Abastecimento do Brasil. Diário Oficial da União 124, Seção 1, pp. 3–4 (2005). [8] Lachenmeier DW et al.: Cancer risk assessment of ethyl carbamate in alcoholic beverages from Brazil with special consideration to the spirits cachaça and tiquira. BMC Cancer 10, 266 (2010). [9] European Food Safety Authority: Ethyl carbamate and hydrocyanic acid in food and beverages, scientific opinion of the panel on contaminants. EFSA J 551, 1–44 (2007). [10] Aylott RI, MacKenzie WM: Analytical strategies to confirm the generic authenticity of Scotch whisky. J Inst Brewing 116, 215–229 (2010). [11] Nóbrega ICC et al.: Ethyl carbamate in pot still cachaças (Brazilian sugar cane spirits): Influence of distillation and storage conditions. Food Chem 117, 693–697 (2009). [12] Caldas NM et al.: Effect of modifiers for As, Cu and Pb determination in sugar-cane spirits by CG AAS. Food Chem 113, 1266-1271 (2009). Proben von Bedarfsgegenständen – risikoorientiert geplant Ein Vorschlag der amtlichen Überwachung in Ostwestfalen-Lippe (OWL) Zusammenfassung Im Jahr 2007 haben Sachverständige der Überwachungsbehörden und der Untersuchungseinrichtung in Ostwestfalen-Lippe (OWL) gemeinsam ein fachliches Konzept zur risikoorientierten Ermittlung der Probenzahlen im Rahmen der Lebensmittelüberwachung vorgelegt, im Jahr 2009 folgte eine Ergänzung für den Bereich der Überwachung kosmetischer Mittel. Bedarfsgegenstände waren bisher noch ausgeklammert. Hiermit wird nun ein ergänzendes Konzept mit einer spezifischen Berechnungsgrundlage für den Bereich der Bedarfsgegenstände vorgestellt. Zentrale Elemente sind die Einteilung der Bedarfsgegenstände in drei Risikogruppen sowie die Zuordnung von Herstellern und Importeuren einer bestimmten Region zu den verschiedenen Arten von Bedarfsgegenständen (Wirtschaftsstrukturdaten). Die jeweiligen Probenzahlen pro Jahr für eine bestimmte Produktgruppe können aus vorhandenen Daten über die Anzahl der herstellenden oder importierenden Unternehmen mit Hilfe eines Produktrisikofaktors und unter Berücksichtigung eines definierten Probensolls berechnet werden. Wie schon in den vorangegangenen Konzepten für Lebensmittel und kosmetische Mittel liegt das Hauptaugenmerk auf Herstellern und Importeuren. Soweit möglich, berücksichtigt das Konzept neben dem Gesundheitsschutz auch den Aspekt des Täuschungsschutzes. Wie schon zuvor für kosmetische Mittel wird auch hier schließlich der vorgegebene Proben- DLR | März 2013 | 109. Jahrgang « » Originalarbeiten 149 [13] European Commission: Commission Regulation (EC) No 2870/2000 laying down Community reference methods for the analysis of spirits drinks. Off J Eur Union L 333, 20 (2000). [14] Lachenmeier DW et al.: Quantification of selected volatile constituents and anions in Mexican Agave spirits (Tequila, Mezcal, Sotol, Bacanora). J Agric Food Chem 54, 3911–3915 (2006). [15] Aylott RI et al.: Ethyl carbamate formation in grain based spirits. Part I: Post-distillation ethyl carbamate formation in maturing grain whisky. J Inst Brewing 96, 213–221 (1990). [16] MacKenzie WN, Clyne AH, MacDonald LS: Ethyl carbamate formation in grain based spirits. Part II: The identification and determination of cyanide related species involved in ethyl carbamate formation in Scotch grain whisky. J Inst Brewing 96, 223–232 (1990). [17] Cook R et al.: Ethyl carbamate formation in grain based spirits. Part III: The primary source. J Inst Brewing 96, 233–244 (1990). Annette Neuhaus1# , Claudia Bindl2 , Helma Haffke3 und Thomas Stuke4 1 Kreis Lippe, Veterinärangelegenheiten und Lebensmittelüberwachung, Felix-Fechenbach-Str. 5, 32756 Detmold 2 Kreis Höxter, Veterinärdienst und Lebensmittelüberwachung, 37669 Höxter 3 Chemisches und Veterinäruntersuchungsamt Ostwestfalen-Lippe, 32717 Detmold 4 Kreis Herford, Veterinär- und Lebensmittelüberwachung, 32045 Herford zahlrahmen, wie er sich aus der AVV RÜb ergibt, kritisch hinterfragt. Dieser Beitrag stellt darüber hinaus ein Schema mit Kriterien zur individuellen Beurteilung der Eigenkontrollsysteme vor. Summary In 2007 experts of competent authorities and laboratory in Ostwestfalen- Lippe (OWL) have mutually offered a specialist concept of a risk based sampling system for the performance of official food control. Cosmetic products and commodities were still excluded. In 2009 followed a corresponding concept for cosmetic products. Hereby a supplementary suggestion is presented with a specific basis for the estimation of samples of commodities including food contact materials. Central elements are the division of commodities into three risk groups as well as a data of the economic structure of a local region, for example the service area of a laboratory. The respective sampling number/ year for one special group of products can be calculated with the knowledge of the number of business operators, who produce or import these kinds of commodities and with a factor for the risk assessment of the # Annette Neuhaus; Tel.: 05231/62-231; a.neuhaus@kreis-lippe.de
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