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

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Chemical composition of whiskies produced in Brazil compared to international products
Summary
Alcoholic strength, volatile acidity, acetaldehyde, methanol, ethyl acetate,
higher alcohols (n-propanol, isobutanol, and amyl alcohols),
ethyl carbamate, and copper were investigated in 7 brands of blended
whiskies produced and bottled in Brazil (BWB) from a wide range of prices,
and two brands of blended Scotch whiskies bottled in Brazil (SWB)
were investigated for comparison. All brands complied with limits established
by Brazilian regulations. The cheapest BWB brand was the most
analytically diverse and the only one containing ethyl carbamate above
the quantification limit, at 0.09 mg/L. When compared to SWB as well as
Scotch, Bourbon, Irish or Canadian whiskies, 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 BWB results.
Zusammenfassung
Alkoholgehalt, flüchtige Säure, Acetaldehyd, Methanol, Ethylacetat, höhere
Alkohole (n-Propanol, Isobutanol, und Amylalkohole), Ethylcarbamat,
und Kupfer wurden in 7 Sorten von in Brasilien hergestelltem und
abgefülltem „Blended Whisky“ bestimmt, die eine breite Preisspanne
umfassen. Zum Vergleich wurden zudem zwei Sorten von in Brasilien
abgefülltem „Blended Scotch Whisky“ analysiert. Alle Produkte entsprachen
den rechtlichen Anforderungen in Brasilien. Interessanterweise
hatte das Produkt mit dem niedrigsten Preis die am weitesten
abweichende Zusammensetzung und enthielt als einziges Produkt auch
Ethylcarbamat mit einem Gehalt von 0,09 mg/L. In Brasilien hergestellter
Whisky hatte, verglichen mit Scotch, Bourbon, Irish und Canadian
Whisky, deutlich geringere Gehalte an Methanol, Ethylacetat, n-Propanol
und Isobutanol. Ein auf dem internationalen Markt nicht üblicher Verschnitt
mit Neutralalkohol kann diese Ergebnisse erklären.
For Table 1 please take a look online:
www.dlr-online.de → DLR Plus
Password: Zentrifugationssäulen
Ian C. C. Nóbrega1# , Sonia P. A. Oliveira1 , Yulia B. Monakhova3 ,
Elainy V. S. Pereira1 , Adelia C. P. Araújo2 , Danuza L. Telles2 ,
Marileide Silva2 , Vera L. A. G. Lima1 and Dirk W. Lachenmeier3 1 Universidade Federal Rural de Pernambuco, Programa de
Pós-graduação em Ciência e Tecnologia de Alimentos,
CEP 52.171-900, Recife, PE/Brazil
2 Laboratório de Agrotóxicos e Contaminantes em Alimentos e
Bebidas Alcoólicas (LabTox), Instituto de Tecnologia de Pernambuco
(ITEP), CEP 50.740-540, Recife, PE/Brazil
3 Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe,
Weissenburger Straße 3, 76187 Karlsruhe/Germany
Introduction
According to data from a large population survey, whisky
is the third most consumed spirit in Brazil [1]. Furthermore,
whisky was the second largest segment of the spirit
market in Brazil in 2010, with sales revenues of US$1.8 billion
[2]. Since in volume terms 65% of the top 9 selling
whisky brands in Brazil are produced and/or bottled in the
country [3], often referred to as “national” whiskies, they
have a large share of this market.
The most relevant type of “national” whisky in Brazil is
the blended whisky. According to Brazilian regulations
[4,5], blended whisky is a spirit drink bottled between
38 % and 54 % alcohol by volume at 20 °C (%vol). The
basic ingredient (min. 30 %) is a spirit (min. 54 %vol;
max. 95 %vol) matured for at least two years in oak casks
(not exceeding 700 litres capacity) and obtained from the
distillation of a malted barley mash (malt whisky). It may
then be blended with aged or non-aged potable ethyl alcohol
of agricultural origin (min. 95 %vol), aged or nonaged
spirit of cereal origin (min. 54 %vol; max. 95 %vol),
water (for alcoholic strength correction), and plain caramel
(for colour correction).
The previous definition implies that blended whiskies produced
and bottled in Brazil (BWB) are in principle not
qualified as whisky under EU regulation [6] for three basic
reasons: (1) use of alcohol that has not been fermented
from cereals; (2) use of alcohol that has not been subjected
# Correspondent: Dr. Ian C. C. Nóbrega, Fax: +558133206260;
ian@dtr.ufrpe.br

146 Originalarbeiten «
to 3-year maturation; (3) use of alcohol that has not been
distilled at less than 94.8 %vol. However, Brazilian regulation
[4] allows imported whiskies to be bottled in the
country if only water and/or plain caramel are added for
final correction. These bottled whiskies may carry the
name of their country of origin on labelling (e. g. “Scotch
whisky”) but still are referred by Brazilians to as “national”
whiskies.
However, contrary to the EU regulation for whisky, the
Brazilian regulation [4] establishes standards for various
congeners and contaminants in whisky, including volatile
acidity (max. 150 mg/100 mL pure ethanol), higher alcohols
(max. 300 mg/100 mL pure ethanol), aldehydes as
acetaldehyde (max. 20 mg/100 mL pure ethanol), esters as
ethyl acetate (max. 150 mg/100 mL pure ethanol), volatile
substances other than ethanol and methanol (congeners,
min. 100 mg/100 mL of pure ethanol for blended whisky),
methanol (max. 20 mg/100 mL pure ethanol), and copper
(max. 5 mg/L).
With respect to the genotoxic carcinogen (IARC 2A) ethyl
carbamate (EC), whiskies are not submitted to any regulation
neither in Brazil nor in the EU. In Brazil the only alcoholic
beverage submitted to an EC control (maximum allowance
of 0.15 mg/L) is cachaça [7], but data from a large
literature survey has shown the spirit to be regularly contaminated
with EC (mean 0.38 mg/L) [8]. However, EC in
whiskies from the EU is apparently under control, since according
to data of the European Food Safety Authority [9]
its average level in 1222 samples from the continent was
0.04 mg/kg (P95 = 0.11 mg/kg), thus below the limit of
0.15 mg/kg established or recommend by several countries
for spirits drinks. EC levels in whiskies produced and/or
bottled in Brazil are unkown.
There have been few publications on the chemical composition
of whiskies produced in Brazil. One exception is a
comparative study by Aylott and MacKenzie [10] on the
chemical composition of whiskies produced in several
countries with Scotch whisky. Although five whisky brands
produced in Brazil were included in the study, products
were not fully described according to their labels [e. g. type
(malt, blended or grain whisky), ingredients, etc.] and
analyses were limited to major volatile congeners (alco-
Erratum
Hofmann H, Patz C-D, Dietrich H:
DLR 107 (11), 575–581 (2012)
Der Titel der Arbeit
„Über den Einfluss von Pektinsäure, CMC und Ascorbinsäure
auf die Farbstabilität von Erdbeerkolloiden“
lautet richtig
„Über den Einfluss von Erdbeerkolloiden, Pektinsäure,
Carboxymethylcellulose und Ascorbinsäure auf die
Farbstabilität von Erdbeersaft“.
Wir bitten den Fehler zu entschuldigen.
holic strength, volatile acidity, ethyl carbamate and copper
were not investigated).
Based on considerations listed above, the aim of this paper
was to investigate EC, copper and major volatile congeners
(acetaldehyde, methanol, ethyl acetate, higher alcohols, and
volatile acidity) in seven brands of blended whiskies produced
and bottled in Brazil (BWB). The results are discussed
in light of Brazilian regulation and the composition is compared
with two brands of blended Scotch whiskies bottled in
Brazil (SWB) as well as with international products from
several countries (Scotch, Bourbon, Irish, Canadian).
Materials and methods
Whiskies produced and/or bottled in Brazil
Duplicate samplings of seven brands (W01–W07) of
blended whisky produced and bottled in Brazil (BWB) and
two brands (W08 and W09) of blended Scotch whisky bottled
in Brazil (SWB) were conducted from a national beverage
distributor/retailer (Imigrantes Mercantil Ltda, www.
imigrantesbebidas.com.br) between May and December
2010. Brand prices (per litre of whisky) ranged from
US$8.35 (W01) to US$15.90 (W09).
Ethyl carbamate, acetaldehyde, ethyl acetate, n-propanol,
isobutanol (2-methyl-1-propanol), iso-amyl alcohol (3-methyl-1-butanol),
methanol, and 1-pentanol were purchased
from Dr. Ehrenstorfer (Augsburg/Germany). Sodium hydroxide
from Merck (Darmstadt/Germany). Copper, palladium
nitrate and magnesium nitrate standard solutions
were purchased from Fluka (Buchs/Switzerland). Ultrapure
water (Milli-Q system) or LC-grade ethanol (Merck,
Darmstadt/Germany) at 40 %vol. was used throughout to
prepare solutions.
The alcoholic strenghts (%volume at 20 ºC) of the spirits
were determined using a Densimat hydrostatic balance
coupled to an Alcomat converter (Gibertini Elettronica,
Milano/Italy).
Volatile acidity as acetic acid was determined using an automatic
DEE Gibertini distillation unit attached to VADE3
Gibertini steam unit (Gibertini Elettronica, Milan/Italy).
Samples (10 mL) were steam distilled, collected (200 mL)
and submitted to titration with NaOH (0.02 mol/L) using
phenolphthalein as indicator. Results were expressed as
mg/100 mL pure ethanol.
EC analysis by Gas Chromatography coupled with Mass
Spectrometry (GC-MS) was carried out as described by our
group previously [11] with some differences: sample injection
and GC column were altered to 1 μL and to a Carbowax
20M (Varian, 60 m × 0.25 mm × 1 μm film thickness),
respectively. The limits of detection and quantification
were 0.01 and 0.05 mg/L, respectively.
Higher alcohols [n-propyl, isobutyl, and amyl alcohols (2-
+ 3-methyl-1-butanol)], acetaldehyde, ethyl acetate and
methanol were determined by a Thermo/Trace GC Ultra
gas chromatograph, using software ChromQuest 4.1,
equipped with flame ionization detector (FID) and Car-
» 109. Jahrgang | März 2013 | DLR

owax 20M column (Varian, 60 m × 0.25 mm × 1 μm film
thickness). An autosampler was used to introduce in splitless
mode 1 μL aliquots of each whisky brand (n = 2). The
GC oven was initially kept at 60 °C, followed by an increase
to 200 °C at 10 °C/min. The temperatures of injector
and detector were set at 230 and 250 °C, respectively.
Quantification was based on calibration curves (analytical
working solutions were prepared in ethanol 40 %vol)
using 1-pentanol as internal standard. Results were expressed
as mg/100 mL pure ethanol.
Cu was determined using a Thermo Scientific GFS 97
atomic absorption spectrometer with deuterium-lamp
background correction, SOLAAR software, equipped with
GFS 97 graphite-furnace/autosampler module. Whisky
samples were introduced directly. Hollow cathode lamps
(Photron, Australia) were used for the determination of Cu
(249.2 nm) operated at 10 mA, according to Caldas, Raposo,
Gomes Neto, and Barbosa [12]. High-purity argon
was used as purge gas throughout at a flow rate of 200 mL/
min. Other operating conditions were carried out according
recommendations of manufacturer. Quantification was
based on calibration curves [analytical Cu working solutions
(0.1–2.0 mg/L) were prepared in ethanol 40 %vol]
and checked by standard addition.
Scotch, Irish, Canadian and Bourbon whiskies
The comparison samples from Europe and North America
were sampled between 2005 and 2011 and analyzed using
the EU reference method [13,14]. For explorative multivariate
data analysis aiming to visualize the data set, the
software Unscrambler X version 10.0.1 (Camo Software
AS, Oslo, Norway) was used. For this evaluation, except
Brazilian samples, 37 Scotch, 6 Canadian, 23 Bourbon and
4 Irish whiskeys were additionally included.
Multivariate analyses
Multivariate evaluation was conducted using principal
component analysis (PCA) based on a data matrix containing
quantitative results for methanol, acetaldehyde, n-propanol,
isobutanol as well as 2- and 3-methyl-1-butanol
from GC. The best PCA results were achieved without any
pretreatment of the data.
Results and discussion
Table 1 shows results for alcoholic strength, volatile acidity,
acetaldehyde, methanol, ethyl acetate, higher alcohols (individually
and combined), ethyl carbamate (EC) and copper
of seven brands of BWB (W01-W07, presented in increasing
order of retail prices per litre of product) and two brands of
SWB (W08 and W09) as well as information about their ingredients
(collected from labels). For comparison with Brazilian
whiskies, Table 1 also shows the analytical results for
Irish, Canadian, Bourbon and Scotch whiskies.
Based on the ingredients provided by labels, all sampled
brands are in principle qualified as blended whisky under
DLR | März 2013 | 109. Jahrgang «
» Originalarbeiten 147
Brazilian regulation. However, most BWB would not be
qualified as whisky under EU regulation since they contain
ethyl alcohol derived from an unspecified source, apart
from malt whisky. In fact, the only brand allegedly containing
ethyl alcohol derived from cereals is W05, but its
alcoholic strength is below the minimum level required
(40 %vol) by EU regulation (Tab. 1).
With respect to alcoholic strength, all brands are in compliance
with Brazilian regulation (min. 38 %vol; max.
54 %vol), but the brands of SWB are additionally in compliance
with the EU regulation.
As seen in Table 1, all sampled whiskies, including the SWB,
comply with the limits established by Brazilian regulation
for whisky (alcoholic strength, volatile acidity, acetaldehyde,
methanol, ethyl acetate, higher alcohols, congeners, and
copper) and the international ethyl carbamate upper limit
(0.15 mg/L) established or recommended by several countries
for distilled spirits in general [9].
With respect to the BWB (W01-W07), results show brand
W01 to be the most analytically diverse. Levels of volatile
acidity, acetaldehyde and methanol in W01 were 120 %,
83 %, and 79 % higher, respectively, than the corresponding
BWB averages. On the other hand, levels of ethyl acetate,
n-propanol, isobutanol and 2- + 3-methyl-1-butanol
in W01 were 25 %, 33 %, 58 %, and 53 % lower, respectively,
than the corresponding BWB averages. Large differences
(W01 compared to other brands) were also observed
in the sums and ratio of higher alcohols (Tab. 1).
To strengthen the analytical distinctiveness of W01, it was
the only sampled brand that contained ethyl carbamate
(EC) above the quantification limit (0.05 mg/L), at
0.09 mg/L still below the international limit (0.15 mg/L).
Research in the early 1990’s showed EC in whisky to be
mainly formed (during- or after distillation) from coppercatalyzed
reactions between ethanol and cyanide related
precursors derived from a cyanogenic glycoside (epiheterodendrin)
present in malted barley [15–17]. As result, the
Scotch whisky industry has taken successful measures to
reduce EC to low levels (usually below 0.05 mg/L) in
whisky since then [9]. It is not known whether producers
of malt whiskies in Brazil have taken any controlling measures,
but the low EC levels found in BWB may also suggest
a dilution effect of EC in the final product by the use
neutral alcohol (essentially ethyl alcohol with very low levels
of congeners and contaminants due to highly rectified
distillation) in the blending process.
Brand W01 was by far the cheapest sampled whisky
(US$ 8.35 per litre of product). Taking into consideration
production costs, results of W01 might reflect the use of relatively
lower proportions of malt whisky in relation to ethyl
alcohol of agricultural origin (often made from cheaper sugar
cane fermentation) in the blending process. Furthermore, as
observed previously in another whisky study by Aylott and
MacKenzie [10], the abnormally low levels of higher alcohols
in W01 (while exhibiting high ratio of 2- + 3-methyl-1-butanol/isobutanol)
can arise from blending malt whisky with
highly rectified ethyl alcohol distilled at >96 %vol.

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

149A Originalarbeiten «
Chemical composition of whiskies produced in Brazil compared to international products
Ian C. C. Nóbrega, Sonia P. A. Oliveira, Yulia B. Monakhova, Elainy V. S. Pereira, Adelia C. P. Araújo, Danuza L. Telles, Marileide Silva,
Vera L. A. G. Lima and Dirk W. Lachenmeier
Tab. 1 Ingredientsa (provided by labels), and analysis resultsb of blended whiskies produced and bottled in Brazil (BWB, W01–W07) and blended Scotch
whisky bottled in Brazil (SWB, W08–W09) as well as Scotch, Irish, Canadian and Bourbon whiskies
Brandc Ingredients Alcoholic
Strength
[%vol]
W01 Malt whisky;
ethanol
W02 Malt whisky;
ethanol
W03 Malt whisky;
aged cereal
spirit; ethanol
W04 Malt whisky;
aged cereal
spirit; ethanol
W05 Malt whisky;
aged cereal
spirit
W06 Scotch malt
whisky;
sugarcane
spirit
W07 Scotch malt
whisky; aged
ethanol
Volatile
acidity
Acetaldehyde
Methanol
Ethyl
acetate
mg/100 mL pure ethanol Ethyl
n-Propanol
(pr)
Isobutanol
(ib)
2- + 3-
Methylbutanold
(mb)
mb/
ibe
pr+
ibf
pr+ib+
mbg
carbamate h
[mg/L]
Cu
[mg/L]
38.5±0.3 58.8±1.0 6.4±1.1 5.2±0.5 10.8±0.4 7.0±0.5 8.9±0.5 34.1±0.2 3.8 15.9 50.0 0.09±0.01 0.3±0.0
39.6±1.0 16.5±0.5 3.1±1.1 2.8±0.0 13.2±0.5 12.2±0.2 20.8±1.9 76.8±2.7 3.7 33.0 109.8 < LQ 0.1±0.0
39.5±0.1 19.7±0.0 2.6±1.7 2.1±0.1 14.4±0.0 10.8±1.1 24.3±1.5 85.8±1.6 3.5 35.1 120.9 < LQ 0.2±0.0
40.4±0.7 18.3±0.2 3.1±0.6 2.1±0.1 14.1±0.0 11.4±0.7 23.8±0.4 83.0±0.4 3.5 35.2 118.2 < LQ 0.2±0.0
38.9±1.2 26.4±0.5 2.3±1.4 4.2±0.3 14.6±0.3 11.7±0.8 23.5±1.7 87.4±0.5 3.7 34.2 122.6 < LQ 0.5±0.1
37.9±0.6 36.2±0.5 4.9±0.6 2.1±0.1 16.0±0.1 10.5±0.6 23.5±0.1 79.4±0.9 3.4 34.0 113.4 < LQ 0.1±0.0
38.9±0.0 21.9±0.1 3.6±0.1 2.6±0.0 21.7±0.2 13.3±0.0 34.2±0.5 100.3±1.3 2.9 47.5 147.8 < LQ 0.2±0.0
Minimum – 37.9 16.5 2.3 2.1 10.8 7.0 8.9 34.1 2.9 15.9 50.0 < LQ 0.1
Average – 39.0 26.8 3.5 2.9 14.5 10.5 21.0 72.6 3.4 31.4 104.1 – 0.2
Maximum – 40.4 58.8 6.4 5.2 21.7 13.3 34.2 100.3 3.8 47.5 147.8 0.09 0.5
W08 Scotch malt
whisky;
Scotch grain
whisky
W09 Scotch malt
whisky;
Scotch grain
whisky
Limits established by
Brazilian regulationsi
Blended Scotch whisky
(n = 32)
Single malt Scotch
whisky (n = 5)
Straight Bourbon
whisky (n = 6)
Blended Bourbon
whisky (n = 17)
42.2±2.4 25.3±1.0 4.2±0.2 6.9±0.5 24.1±0.6 46.1±0.8 52.8±0.8 77.7±4.4 1.5 98.9 176.6 < LQ 0.1±0.0
39.9±0.0 35.8±0.2 4.7±0.8 5.1±0.0 27.4±0.9 54.7±1.2 57.1±0.2 95.4±3.1 1.7 111.8 207.2 < LQ 0.2±0.0
38-54 0-150 0-20j 0-20 0–150k – – – – – 0–300l – 0–5
39.8±0.2 m 5.1±2.0n 6.8±3.0 m 64.0±18.7 56.6±7.5 55.8±22.8 1.0 120.6 176.4 m m
40.9±2.6 m 15.9±2.7 6.3±0.6 m 46.7±2.9 78.9±9.0 209.3±15.4 2.7 125.6 334.9 m m
40.4±1.7 m 8.6±4.3 14.1±1.2 m 28.7±3.8 155.1±8.9 402.8±61.9 2.6 183.8 586.6 m m
39.7±0.1 m 8.3±1.5 14.1±1.8 m 20.9±2.8 73.9±7.7 302.6±24.4 4.1 94.8 397.4 m m
Irish whisky (n = 4) 39.9±0.2 m 7.9±2.3 8.2±0.5 m 28.4±7.6 21.1±8.2 70.0±21.6 3.3 49.5 119.5 m m
Canadian whisky (n = 6) 39.9±0.4 m 2.5±0.9 6.6±3.2 m 10.2±12.7 5.3±2.5 12.4±4.1 2.4 15.4 27.8 m m
a Basic ingredients only. Although water (for alcoholic strength correction) and caramel (for colour correction) are listed ingredients in all brands they are not shown in Table 1.
b Values are expressed as average ± standard deviation c Brands are ranked in increasing order of retail prices per litre of product in Brazil. d Peaks of 2-methyl-1-butanol and
3-methyl-1-butanol (amyl alcohols) co-eluted. e Amyl alcohols/isobutanol. f n-propanol + isobutanol. g n-propanol + isobutanol + amyl alcohols. h Limit of quantification (LQ) of ethyl
carbamate = 0.05 mg/L;