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Chemical composition analysis and authentication of whisky

Article in Journal of the Science of Food and Agriculture · November 2014

DOI: 10.1002/jsfa.6960

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CHEMICAL COMPOSITION ANALYSIS AND AUTHENTICATION OF

WHISKY

Paulina Wiśniewska*, Tomasz Dymerski, Waldemar Wardencki, Jacek Namieśnik

*
p.m.wisniewska@gmail.com

Department of Analytical Chemistry

The Chemical Faculty

Gdansk University of

Technology 11/12 Narutowicza

St.

80-233 Gdansk, Poland

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may lead to differences between this version and the Version of Record. Please cite this
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reserved
 ABSTRACT

Whisky (whiskey) is one of the most popular spirit-based drinks made from malted or

saccharified grains, which should mature for at least three years in wooden barrels. High

popularity of products usually cause a potential risk of an adulteration. Regarding to that

fact the authenticity assessment is one of the key elements of food product marketing.

Authenticity of whisky is based on the comparison of composition of this alcohol with

other spirit drinks. This paper summarizes all information about the comparison of whisky

and other alcoholic beverages, the identification of type of whisky or the assessment of its

quality and finally the authentication of whisky. The work also presents the various

analytical techniques for analyzing whisky such as: gas and liquid chromatography with

different types of detectors (FID, AED, UV-Vis), electronic nose, atomic absorption

spectroscopy and mass spectrometry. In some cases the application of chemometric

methods there are also described, namely: PCA, DFA, LDA, ANOVA, SIMCA, PNN, k-

NN, CA, and preparation techniques such SPME or SPE.

Keywords: whisky, authentication, chromatography, food analysis, e-nose

INTRODUCTION

Whisky (whiskey) is one of the most popular spirit-based drinks. Depending on the region,

whisky is defined differently. According to the European definition of whisky, it is a spirit

drink produced via distillation of mash made from malted grains or from grains which have

been saccharified by the diastase of the malt contained therein. Distillation is conducted at

less than 94.8 % vol. in order to retain an aroma and taste derived from the raw materials

used. Whisky should mature for at least three years in wooden barrels of a capacity not

exceeding 700 liters. The final distillate retains its color, aroma and taste derived from the

production process. Only water and plain caramel (for coloring) can be added to the

distillate; no other colorings and flavorings can be added. Scottish whisky is the most

popular whisky
type. It is produced entirely from malted barley via double distillation in large copper pot

stills. The volatile phenolic compounds, inter alia, cresol and guaiacol that form in roasted

barley are responsible for the specific taste of whisky. Whisky originating from the

northern part of the USA is made from the mixture of corn, rye, wheat, barley and other
1-4
grains. It is aged in oak barrels for at least two years .

Allegedly, whisky originated in Ireland where local monks were already producing distilled

alcohol known in Latin as aqua vitae (translated to Gaelic as uisge beatha) in the 7th

century. It was a mixture obtained via distillation of fermented fruits, and used for

medicinal purposes only. In the 17th century, the shortened name uiskie started to be used,

while in 1715, the name was changed to whiskie. The present-day name “whisky” was

established in 1736. In the 9 th century, the Irish monks and their medicinal alcohol reached

Scotland. Information about the water of life made from barley appeared in the mid-16th

century. At the turn of the 18th century, the British Parliament taxed the production of

whisky, which resulted in a decrease of legal production and, obviously, an increase in

illegal production of this spirit. These circumstances stimulated the development of diverse

whisky types produced by small camouflaged distilleries, and the use of traditional recipes

passed on through the Scottish clans. As a result of this natural diversification, three types

of whisky exist presently, i.e. blended whisky, grain whisky and malt whisky. Blended

whisky, produced via mixing of grain whisky and single malt whisky, is represented by the

brands such as, Johnny Walker and Ballantine's. Grain whisky is made from the mash

consisting of different grains, mostly of barley, wheat and corn. It is produced via

continuous distillation in a column still. Actually, the only difference between grain whisky

and vodka is that the former has to be aged for three years in an oak barrel. Grain whisky

made from one type of grain, so-called single grain whisky, is also produced. In this case,

either malted or unmalted barley can be used. Malt whisky is made from malted barley. Its

distillation takes place in copper pot stills,

followed by maturation in oak barrels usually for over 8 years. Malted whiskies can be

divided into two groups, i.e. single malt whisky (malted whisky originating from one

distillery) and vatted malt whisky (a blend of single malt whiskies originating from

different distilleries) 5.

This article presents the methods for analyzing whisky composition which also enable its

authentication. The chemical composition analysis can be conducted be means of, inter

alia, chromatography and spectrometry as well as other techniques. The application of the

aforementioned methods enable authentication, the determination of exact composition,

and quality evaluation of whisky. Thanks to these procedures, it is possible to remove

falsified products from the market, and to select a whisky which will fulfill expectations.

ANALYSIS OF WHISKY COMPOSITION

Each spirit has a characteristic aromatic profile, which influences the processes of

fermentation, distillation and storage as well as the selection of an appropriate raw material.

The compounds responsible for the aroma are, e.g. fusel alcohols, fatty acids and esters.

Spirits are a diverse group therefore in order to determine individual qualities of a given

alcoholic beverage, it is necessary to determine its composition. Studies on the exact

composition of whisky are mainly performed by using gas chromatography. Such research

allows for finding characteristic compounds and defining aroma profiles, which can then be
6
used for defining the quality and authenticity of the tested whisky. Fitzgerald et al.

analyzed Scotch and Irish whiskies by means of gas chromatography coupled with a mass

spectrometer (GC-MS). Samples were prepared by solid-phase microextraction (SPME).

Solid-phase microextraction (SPME) is based on the sorption of small amounts of samples

onto a thin cylindrical layer of stationary phase coating the glass or quartz fiber. The fiber

is placed inside the rust-free tube that is located in the syringe needle. Such set-up enables

the mass exchange during the enrichment and release of the adsorbed compounds, and

prevents
clogging. The extraction can be conducted by immersing the fiber directly in the liquid (DI

– SPME) or by placing it in the head space above the liquid or solid sample (HS – SPME) 7,
8
. The applicability of three fiber types was tested, namely, PDMS-DVB, CAR-PDMS and

PA, the latter being the most suitable for the procedure. Seventeen compounds were

selected for the analysis, including fusel alcohols, acetates and esters; however, the

concentration levels of six of them turned out to be below their detection limits in all

samples. Despite this situation, the applied technique was useful for quantitative analysis of

the selected compounds in whisky samples 6. This research allowed for defining a useful

method, which can then be used for analyzing compounds characteristic of whisky. Poisson
8
and Schieberle analyzed the composition of American Bourbon by applying High

Resolution Gas Chromatography – Olfactometry (HRGC-O). This technique allowed the

detection of 23 active aroma substances. Based on the review of previously published data,

it turned out that 13 of these compounds were never detected before, i.e. ethyl (S)-2-

methylbutanoate, (E)-2- heptenal, (E,E)-2,4-nonadienal, (E)-2-decenal, (E,E)-2,4-

decadienal, 2-isopropyl-3- methoxypyrazine, ethyl phenylacetate,

4-methylacetophenone, α-damascone, 2-phenylethyl propanoate, 3-hydroxy-4,5-dimethyl-

2(5H)-furanone, trans-ethyl cinnamate, and (Z)-6-dodeceno-γ-lactone. Thanks to the use of

olfactometry, it was possible to assign concrete aromas to the identified compounds 9. The
10
next article by Poisson and Schieberle was a continuation of previous research and

included the quantitative analysis of 31 compounds selected from among the substances

which had already been detected via two-dimensional high resolution gas chromatography

coupled with a mass spectrometer (TD-HRGC-MS). The results obtained were used to

formulate the aroma characteristic for American Bourbon by mixing 26 compounds at

specified concentrations with the solution of water and ethanol 10. An aroma profile of this

kind can be used to differentiate American Bourbon from other kinds of whisky.
Multidimensional gas chromatography coupled with mass spectrometry and olfactometry
11
(MDGC-MS-O) was used by Wanikawa et al. to identify green note compounds in malt

whisky. These compounds are characteristic of some kinds of whisky, which means that

they can be helpful in the assessment of the authenticity of tested products. The applied

technique allowed the detection of two aldehydes (i.e. E-2-nonenal and E,Z-2,6-

nonadienal) and three alcohols (1-octen-3-ol, 4-hepten-1-ol, nonan-2-ol) which are

responsible for the green note aroma. It was demonstrated that the green note whisky
11
contains more aldehydes and nonan-2- ol compared to other whisky types . Besides the

attempts of identifying the exact composition of the volatile fraction in whisky, the

investigations of chosen groups of compounds and single compounds were conducted. It is

noted that some groups of compounds have greater influence on the aroma of whisky.
12
Esters are an example of such a group. Camp et al. used two-dimensional gas

chromatography coupled with the mass spectrometer (GC-GC-MS) in order to

12
analyze ethyl esters in whisky . These compounds mainly form during the

fermentation and aging processes. Esters are characterized by intense aroma and the low

value of odor detection threshold. Depending on the concentration of esters, they may have

a positive or negative effect on the aroma of an alcoholic beverage. For example, ethyl

acetate at high concentrations gives solvent-like or vinegar note to the final product, while

at low concentrations, it softens the sharp aroma of other beverages 13. Because of that it is

of utmost importance to quantitatively analyze this group of compounds. In order to

preconcentrate the analyzed compounds in samples, solid phase extraction was used (SPE)
12
.

14
Haloanisoles were another group of compounds studied by Campillo et al. . These

compounds form in whisky aging in oak barrels. Their monitoring may enable an

assessment of the ageing process and, as a result, verification of the authenticity of the age

of whisky. The study results demonstrated that solid-phase microextraction coupled with
gas
chromatography and atomic emission detection (SPME-GC-AED) is a perfect system for
14
monitoring the contents of 12 selected haloanisoles . A class of phenols is among the

compounds investigated in whisky. This is connected with their different contents in

individual types of whisky. Twelve substances belonging to phenols were analyzed in the

samples of whisky originating from Scotland (15), Ireland (1), USA (4), Canada (1), Japan

(5), Spain (1), Argentina (1), New Zealand (2) and India (1) by using GC-MS. As a result,

2,4-dimethylphenol was detected in the volatile fraction of whisky for the first time. The

main difference between the samples from specific countries was in the concentration of o-,

m- and p-cresol. The highest concentration of these compounds was determined in whisky

from Scotland. Moreover, the samples of Scottish, Canadian and Bourbon whisky were

compared. The highest concentration of phenols was found in Scottish whisky, while the

lowest one, in Canadian whisky. On the other hand, the highest concentration of eugenol

was observed in Bourbon whisky 15. It is concluded from this article that an analysis of the

presence of selected phenols and their total amount can be used for distinguishing whisky

according to its geographical origin. Apart from selected groups, also individual

compounds are analyzed with the presence being characteristic of selected spirits. Among
16 17, 18 19
the analyzed single compounds were γ-lactone , ethyl carbamate and methanol .

Lactones are well- known organic compounds which display diverse biological effects, e.g.

anticancer, antiviral, antibacterial and anti-inflammatory activities, etc. Lactones have also

been recognized as the components of taste and aroma in alcoholic beverages, mainly in

whisky, wine and cognac. The characteristic odor of the famous Japanese sake results from

the presence of sotolon 20. γ- lactones are responsible, to a large extent, for the aroma of
16
whisky. Wanikawa et al. conducted a study whose aim was to identify the compounds

responsible for “sweet” and “fatty” aromas in malt whisky from Scotland. The analysis was

performed by using GC-MS and GC-O. It has been determined that γ-decalactone and γ-

dodecalactone are responsible for

 16
“sweet” and “fatty” aromas, respectively . Ethyl carbamate is another compound which

should be analyzed in alcoholic beverages. This is needed due to its influence on the quality

of the product. Ethyl carbamate (EC) is a natural compound that occurs in fermented foods

and alcoholic beverages such as, bread, yoghurt, soy sauce, wine, beer, and particularly in

spirits made from stone fruits and stone-fruit pomace (e.g. cherry, plum, mirabelle plum

and apricots). Research has demonstrated that ethyl carbamate has a carcinogenic effect in

laboratory animals. The International Agency for Research on Cancer has classified EC as
21, 22
possibly carcinogenic to humans . Ethyl carbamate was analyzed in alcoholic

beverages, inter alia, in whisky by means of gas chromatography coupled with tandem

mass spectrometry (GC/MS-MS). The technique was tested for its suitability to determine

low concentrations of EC. Five samples of whisky were analyzed; the detected level of

ethyl carbamate varied from 60 to 330 ppb 17. EC was also analyzed in Scottish whisky by

using GC-MS. Five types of blended whisky, including two deluxe and two malt whiskies,

were investigated. A total of 229 samples were processed. The mean concentrations of

ethyl carbamate in specific whisky types were similar, except for deluxe whisky which had

higher EC content 18. Methanol is similar in this respect. This is also a toxic compound,

which must be monitored due to its influence on the quality of whisky. The presence of
19
methanol was investigated by means of an electronic nose . The electronic nose is an

analytical device used for the fast detection and identification of odorant mixtures; its mode

of operation mimics the human sense of smell. The electronic nose employs specific

chemical sensors which generate a characteristic aroma profile, a so-called fingerprint, in

response to being exposed to the investigated gaseous mixture. The identification of

mixture components is based on the comparison with reference profiles 23. Wongchoosuk et
19
al. used the electronic nose equipped with carbon nanotubes (CNT) to investigate the

samples of whisky tainted with different amounts of methanol. Principal component

analysis (PCA) was used to analyze

the obtained data. The principal component analysis (PCA) is based on transformation of

the original variables to new variables. The PCA provides a rotation of the coordinate

system to maximize the variance of the all the coordinates. The PCA is mainly used to
24
model, compress and visualize data . The applied method allowed the graphical

identification of methanol- free whisky and whisky containing methanol at four different

methanol concentrations. Distinguishing among specific methanol concentrations in the

19
samples was also possible thanks to the application of PCA . Besides the concentrations

of organic compounds, the contents of zinc, lead and copper ions was also determined. The

presence of inorganic compounds is tested in connection with the quality of whisky as they

can also influence its aroma. Anodic stripping voltammetry (ASV) and atomic absorption

spectrometry (AAS) were employed in this study. In the case of whisky samples, ASV

turned out to be a more suitable method because it allowed the detection of all analyzed

ions in all samples 25.

A COMPARISON BETWEEN WHISKY AND OTHER ALCOHOLIC BEVERAGES

Being one of the most popular alcoholic beverages, whisky is often compared with other

known spirits in relation to chemical composition. Such studies aim at establishing whether

different types of spirits can be identified by means of analytical techniques. For example,
26
Cardeal and Marriott describe how cachaça, whisky, rum, vodka, gin, tequila and

selected liqueurs were identified by using two-dimensional gas chromatography. The

specification of compounds present in the sample matrix was prepared for cachaça and rum

only. Whisky and other spirits were compared based on the obtained chromatograms. In

comparison to other spirit-based beverages, whisky and vodka had the poorest

chromatographic profiles. Compounds belonging to alcohols, aldehydes, ketones, terpenes,

aromatic compounds, esters and acids were detected in the samples of whisky. The

chromatogram representing whisky is very poor in comparison to other obtained

26
chromatograms . The electronic nose was also used to compare different alcoholic
beverages 27. There are electronic noses which combine
the features of fast gas chromatography with the properties of an electronic nose. One

analysis conducted with such device supplies concurrent information about the sample

composition and the profiles of volatile fractions. Thanks to this, complete information

about the similarity between the given sample and reference sample is obtained. The

electronic nose coupled with fast gas chromatography was used to distinguish among

vodka, tequila, whisky, beer and wine. The statistical analysis was performed by using

principal component (PCA) and discriminant function analysis (DFA). Discriminant

function analysis is used for determining which variables allow for the best division of a

given group of cases on naturally occurring groups. Discriminant function analysis is used
28
for classification of samples to previously defined groups . The DFA method gave better

results because it allowed for distinguishing the types of alcoholic beverages, including
27
four whisky brands . Apart from comparing alcohols in relation to entire matrices,

research was also conducted as regards the comparison of the content of only some groups

of compounds. Ng et al. 29 analyzed selected acids and phenols (a total of 19 compounds) in

whisky and cognac samples by means of GC- MS. Moreover, five compounds, i.e. vanillin,

syringaldehyde, coniferaldehyde, gallic acid and vanillic acid were determined in samples

of spirits of different age. In the case of Scotch whisky, the chosen samples were 12, 17 and

30 years old. The other sampled whiskies were 6 and 12 years old. In general, the samples

of oldest whiskies contained the highest concentrations of the analyzed compounds.

However, in the case of Scotch whisky, one sample of 17-yr old spirit has lower

concentration of coniferaldehyde than that measured in the sample of 12-yr old spirit. This

indicates that the relationship between the age of whisky and the content of phenolic

compounds is not a simple one 29.

IDENTIFICATION OF WHISKY WITH REGARD TO ITS TYPE, QUALITY,

BRAND AND ORIGIN

Due to the high diversity of alcoholic products, the assessment of whisky with regard to its
30
brand, quality and origin is necessary. The study conducted by Lehtonen et al. by means

of GC-FID and UV-Vis can serve as an example here. The obtained data were analyzed by

PCA method. The investigations were conducted twice by using different UV-Vis

techniques. At first, HPLC with UV-Vis detection was applied; the absorbance was

measured in the wavelength range from 220 to 520 nm. The concentrations of propanol,

isobutanol, 2-methyl- 1-butanol and 3-methyl-1-butanol were determined by means of GC-

FID. The samples of whisky originating from Canada (2), Finland (3), Ireland (1) and

Scotland (8) were analyzed. Besides whisky, the samples of rum and brandy were also

investigated. The results of UV- Vis measurements did not supply sufficient information to

distinguish among the whisky samples with regard to the country of their origin. The

second set of measurements encompassed the absorbance determinations at a wavelength

of 380, 440 and 500 nm made with a spectrophotometer, and the concentration

measurements of the aforementioned compounds and methanol. The samples of whisky

from Canada (2), Ireland (10) and Scotland

(15) were analyzed. As in the previous case, the UV-Vis analysis alone was not sufficient

to distinguish among the processed samples. This has become possible thanks to the
30
application of PCA to the results of GC-FID analysis . Gas chromatography combined

with numerous chemometric analyses is used for the analysis of whisky according to its

geographical origin. Three types of whisky, i.e. Scottish, Irish and Bourbon were

distinguished by means of GC- MS and different statistical methods. González-Arjona et al.

31
stated that the best results were achieved with kNN, PDA, MLP and PNN methods. The

kNN algorithm belongs to the group of algorithms, in which the description of the

classifier's target function is not performed during the classifier's training, but at the stage

of assigning an object to the specific classes. The underlying principle of the classifier's

operation is that the object belonging to a specific class has in its close proximity other
objects belonging to the same
class. Classification in performed by comparing the fitted object to all objects stored in the
32,
training set and then choosing from among the key defined k objects that are most alike
33
. Artificial neural network involving multilayer perceptrons (MLP) is a multilayer one-

directional neural network. They are the most frequently used kind of ANN. An artificial

neural network mimics a biological neural network, which collects and transfers signals to

the central nervous system, processes the data, and makes specific decisions depending on

the identified objects. The basic elements of artificial neural networks are artificial neurons
33, 34
. Probabilistic neural networks (PNN) are a kind of artificial neural networks capable of

independent learning. When a new teaching standard, which may introduce additional

information of very important nature, becomes available, it is not necessary to start the

learning process from the beginning. It is possible to introduce such a new standard directly

into the network in the form of another radial neuron. This feature is very significant as it
32,
allows the continuous operation of a PNN without any breaks for a long learning process
33 35
. The same whisky types were analyzed by González-Arjona et al. by means of GC-MS.

The data were processed by PCA and CA methods. Cluster analysis is a method, which

allows for grouping elements described by more than one feature into relatively

homogenous classes. The most important part of CA is the formation of clusters, that is, the

sets of objects where the similarity between any two objects from the same set is higher

than that between any other object from the same set and any object not belonging to the

set. The clusters do not overlap, i.e. none of the objects can belong to more than one class.

The clusters are separated by a precisely determined distance, which can be defined in a

number of ways 33, 36. The contents of 1-propanol, 2-methyl-1-propanol, 3-methyl-1-butanol

and 2-methyl-1- butanol were determined in the samples of 12 Irish whiskies, 20 Bourbons,

and 26 single malt Scottish whiskies. Thanks to the combined use of GC-MS technique and

PCA method, it was possible to distinguish among all the analyzed samples. Irish whiskies

were the most compact

group in the PCA graph which demonstrates that the four compounds selected for the

analysis are enough to distinguish Irish whisky from other whisky 35. Apart from verifying,

whether it is possible to define the county, from which whisky originates, tests were

performed aimed at verification as to whether it is possible to determine the region of

37
origin of a given whisky. Mignani et al. analyzed 18 samples of Scotch whisky, which

included 15 samples of single malt whisky (10 samples from the uplands, and six samples

from the islands) and three samples of blended whisky. Each analyzed whisky was of

different brand identity. The samples were investigated by means of optical spectroscopy,

while the obtained data were analyzed by PCA and LDA methods. Linear Discriminant

Analysis (LDA) is a statistical method, which allows division into border areas by means of

linear functions and works well in data analysis. This is one of the data classification

methods. Such methods are aimed at determining class allocation of other tested objects
33, 38
described by the same or similar chemical structural features . The applied

methodology allowed distinguishing among various whisky types, i.e. blended whisky was

distinguished from single malt whisky. However, it was problematic to divide the samples

based on the region of their origin. In the case of whiskies originating from the uplands and

islands, one sample in each region poorly fitted to the model 37. In order to determine the

region of sample origin and sample type, Adam et al.

39
attempted to use atomic absorption spectroscopy (AAS). Thirty-five samples of whisky

were analyzed; the samples differed with regard to distillery, the region of origin, whisky

type and vintage. The contents of copper, zinc, lead, nickel, iron, calcium, magnesium and

sodium were determined in the samples. The obtained data were statistically analyzed by

means of CA. It was demonstrated that the origin of whisky cannot be identified based on

the contents of the aforementioned compounds. However, malt whisky had much higher

concentration of copper than blended Scotch and pure grain whisky. This finding shows

that a simple analysis of copper content may allow distinguishing malt whisky from other
whisky
 39
types . Various kinds of whisky and brandy were compared based on the ratio of

2-methylbutanol to 3-methylbutanol by using the GC-FID technique. The analyzed whisky

samples included blended whisky (14), malt whisky (14), Bourbon (2), Canadian whisky

(2) and whisky originating from Denmark (3). The highest and the lowest content of both

analyzed compounds was determined in Bourbon and Danish whisky, respectively. The

ratio of 2-methylbutanol to 3-methylbutanol ranged from 0.32 to 0.44. Only two samples

had ratios of 0.32 and 0.33, while the ratio values for the remaining samples were greater

than

0.36. This allowed distinguishing whisky from brandy because the ratio values in brandy

ranged from 0.19 to 0.33 40. Apart from testing the origin and kind of whisky, tests were

performed to distinguish between whiskies of the same kind produced by various brands.

Three well-known whisky brands, i.e. Black Label, Ballantine's and West Highlands were

analyzed by means of GC-MS, including sample preparation by SPME technique. The

microextraction technique was optimized with regard to the fiber type; CAR/PDMS fiber

has been selected from among the five evaluated fibers. The compounds detected in whisky

samples belonged to monoterpenes, higher alcohols, esters, fatty acids, carbonyl

compounds and phenols. Differences detected between specific whisky brands were mainly

of quantitative nature. In all analyzed samples ethyl esters were the most numerous group

of compounds. In the case of higher alcohols, it was observed that the concentration of 3-

methyl-1-butanol in Black Label whisky was definitely higher than that in other whisky

brands. The concentration of carbonyl compounds showed a similar pattern. The lowest

concentration of terpenes was determined in Ballantine's whisky. By using the sum of the

areas under the peaks attributable to specific compounds, it was possible to distinguish
41
among specific whisky brands . Apart from the aforementioned research, it was also

checked as to whether it was possible to distinguish between whiskies of different quality.

Such tests would be helpful in verifying the authenticity of high-quality whisky, which is
often counterfeited with poorer-quality whiskies. In order to distinguish among Scottish

whiskies of different quality, a sensory evaluation and various statistical methods (PCA,
42
ANOVA and PLS regression) were employed by Lee et al. . Analysis of variance

(ANOVA) is a parametric tool that allows for comparing more than two groups, which had

been categorized based on one variable (one-way ANOVA). The underlying idea is to

compare the variance of dependent variables within the groups that had been created, based
33, 43
on the values of independent variables . The partial least squares method (PLS)

combines features of principal component analysis and multiple regression. First, a set of

latent variables is distinguished, which explain as much covariance as possible between

independent and dependent variables. Next, at the regression phase, values of dependent
44
variables are predicted using independent variable decomposition . The samples of

blended whisky were divided in the following categories: deluxe (11), standard (22),

multiple retailer (4), and West Highland (3). PLS regression turned out to be the best

method for data analysis because it correctly grouped all types of whisky, except for the

West Highland type. The dominant aroma of Deluxe whisky was described as fruity,

buttery, malty and nutty, and also vanilla, floral, pungent, sweet and smooth. The aroma of

retailer whisky was evaluated as solventy, soapy, rancid, grassy, mouldy, pungent, grainy,

oily and spicy. The dominant organoleptic qualities of standard whisky were characterized

as oily, sulfury, rancid, grainy, smooth, soapy, vanilla, solvent and sweet. West Highlands

whisky was described as woody, smoky, spicy, medicinal and sulphurs, mouldy, pungent,

soapy and malty notes 42. Similar research aimed at distinguishing among blended whiskies

of different quality was conducted by Lee et al. 45. The whisky samples were analyzed by

using SPME-HRGC-MS, while the obtained data were processed with the same statistical

methods as before, i.e. PCA, ANOVA and PLS regression. A total of 38 compounds was

analyzed. Deluxe whisky was identified based on the contents of ethyl hexanoate, ethyl

heptanoate, ethyl acetate, ethyl nonanoate,

ethyl decanoate, isoamyl decanoate and isoamyl hexanoate. The content of acetate esters

(dodecyl and phenylethyl esters, and 3-methylbutyl acetate) was used to identify standard

whisky. In the case of retailer whisky, ethyl hexadecanoate, ethyl octadecanoate, ethyl

tetradecanoate and propyl decanoate were the markers. West Highlands whisky was

identified by the presence of furfural, isobutyl octanoate and ethyl benzoate 45.

AUTHENTICATION OF SCOTCH WHISKY

Scotch whisky the most highly valued of spirits that is preferentially chosen by consumers.

It is produced almost exclusively in Scotland from malted barley or barley; Scotch whisky

is aged in wooden barrels for three years. The most popular scotch brands are Johnie

Walker, Teacher’s, The Famous Grouse, Chivas Regal, Laphroaig, The Balvenie and

Ballantine’s. The name “Scotch whisky” is a geographical indication assigned to Scotland;

the term is protected by international law. Genuine Scotch whisky has to be produced in

Scotland therefore the authentication of this spirit is of utmost importance. Scotch is the

most frequently falsified whisky thusScotch numerous studies on the methods of its
46
authentication have been published. Parker et al. used gas chromatography-combustion-

isotope ratio mass spectrometry (GC-C-IRMS) to authenticate whisky. Eight samples of

popular Scottish whisky and two samples of other whisky types were compared. The

carbon isotopic ratios were analyzed for selected congeners, i.e. acetaldehyde, ethyl acetate,

n-propanol, isobutanol and amyl alcohol. The plotted graphs allowed distinguishing among

the analyzed samples, and finding the samples of falsified spirits 46. Scotch whisky was also
47, 48
authenticated by means of GC-MS and HPLC . It became apparent that the analysis of

higher alcohols is the most important part of such authentication procedures. Higher

alcohols are the most representative group attributable to whisky, particularly n-propanol,
47 48
isobutanol and amyl alcohol . In the second article , a number of qualities had been

defined which scotch whisky should posses. These qualities include, inter alia, the alcohol

content not lower than 40%; methanol content

lower than 25 g / 100 l; the sum of the contents of n-propanol and isobutanol at least 97

g/100 l; the ratio (sum of 2-methylbutanol and 3-methylbutanol)/ 2-methylbutanol not

lower than

1.9 and not higher than 3.5; and the ratio of 3-methylbutanol to 2-methylbutanol not lower

than 2.2 and not higher than 3.5. All the aforementioned properties allow the authentication
48 49
of Scottish whisky . MacKenzie and Aylott decided to check whether the UV-Vis

technique can be used to authenticate whisky produced in Scotland. To this end, 35 samples

were analyzed of which 20 were suspected to be Scottish whisky and the remaining 15

samples to be other whisky types. In order to confirm the UV-Vis results, gas

chromatography was also used as it has been previously assessed as suitable for the

authentication of Scottish whisky. According to chromatographic analysis, only eight

samples were classified as Scotch whisky and one sample was considered suspicious.

Based on the UV-Vis analysis, seven samples were classified as Scotch whisky (agreement

with GC analysis), one as falsified (disagreement with GC), and one sample as suspicious
49
(different sample than the one pointed to by GC) . Ashok et al. and Backhaus et al.

undertook the task of assessing whether near-infrared spectroscopy (NIRS) is suitable for
50, 51
analyzing Scotch whisky . Different brands of Scottish whisky were analyzed with

regard to taste, age and barrels in which they had been aged. The data obtained were

processed by PCA and PLS regression. The spectroscopic spectrum of whisky mainly

represents ethanol due to the high content of this compound in the sample. Besides ethanol,

whisky contains other alcohols, esters, aldehydes and organic acids, called congeners. The

presence of these compounds allows the identification of the brand, age and quality of a

given sample. However, it is only possible based on the comparative analysis of

fluorescence background of the spectra. This technique combined with chemometric

analysis enables the fast evaluation of whisky quality. The samples differing with regard to
50
brand, age and barrel type can be properly grouped by using NIRS and PCA . The
falsified Scotch whisky was also detected by employing mid-
infrared spectrometry. A total of 17 samples analyzed which included falsified and genuine

Scotch whisky. The study concerned the ethanol concentration and colorants used. The

obtained data were statistically analyzed by PCA and PLS regression. Seven samples were

classified as falsified because their ethanol content was below the required standard value

of 40%. One sample was on the borderline of statistical significance therefore it had been

temporarily classified as genuine. The next stage of the study dealt with testing for the

presence of commercially available colorants among which only one is authorized. Based

on the obtained results, eight samples were classified as genuine Scotch whisky, while the

rest of the samples were recognized as falsified. A comparative analysis of both data sets

demonstrated that only seven samples fulfilled both requirements and thus could be
52
considered genuine Scotch whisky . As previously mentioned, only whisky produced in
53
Scotland can be called Scotch whisky. Meier-Augenstein et al. undertook the task of

evaluating the applicability of High Temperature Conversion-Isotope Ratio Mass

Spectrometry (TC/EA-IRMS) technique for determining the origin of whisky. To that end,

the samples of water used in the whisky production and genuine whisky from all Scottish

distilleries as well as samples of falsified Scotch, the latter supplied by the Scottish Whisky

Research Institute (SWRI), were analyzed. TC/EA-IRMS allowed for distinguishing

between the falsified and genuine whisky which suggests that the applied analytical

technique can be used for confirming the authenticity of geographical origin in whisky

samples 53. Garcia et al.

54
analyzed 80 samples of whisky, namely, 50 samples of authentic brands of Scottish whisky

and 30 samples of falsified Scotch by using Fourier transform ion cyclotron resonance

mass spectrometry (FT-ICR MS). The obtained data were statistically analyzed by the PCA

method. At first, a comparative analysis of authentic whisky brands was performed to

determine whether it is possible to distinguish among them. Two brands, i.e. Buchanan’s

and J&B were found to be easily identifiable. Red Label, Black Label and White Horse
were
located closely together and even slightly overlapping in the graph which can cause

problems with a very precise identification of these brands. The second part of the analysis,

described in the same article, dealt with distinguishing between the authentic and falsified

whisky samples. The application of the FT-ICR MS technique and the PCA method

demonstrated that all authentic whiskies were grouped together in the graph, while the

falsified whiskies were farther away from them. These findings prove that the applied

technique is also suitable for the authentication of Scottish whisky 54. Yet another method

capillary electrophoresis was evaluated as a possible technique for the authentication of

Scottish whisky; LC-MS/MS was employed as a comparative technique in this study. A

total of 32 samples was analyzed which included 10 reference samples, 21 samples of

possibly falsified spirits, and one sample of whisky purchased in the local supermarket. The

samples were of different vintage. The contents of syringaldehyde, vanillin, sinapaldehyde

and coniferaldehyde were determined. For all samples classified as falsified,

syringaldehyde, sinapaldehyde and coniferaldehyde were present at concentrations below

the detection limit, while vanillin concentration was lower than in the samples of authentic

whisky 55. The samples of genuine Scottish (11 samples) and American (2 samples) whisky

were compared to the falsified Brazilian whisky (2 samples) by means of electrospray

ionization mass spectrometry (EI-MS). The obtained data were analyzed by discriminant

partial least square (D-PLS) regression. The analysis demonstrated that the used technique

allowed for distinguishing among Sottish, American and Brazilian whiskies. However, a

distinction between Scotch blended whisky and Scotch single malt whisky was

questionable 56.

SUMMARY

Whisky, being one of the most popular alcoholic beverages, is researched very often. Such

investigations are conducted as a result of high diversity and widespread production of this

spirit. Scotch whisky is widely appreciated by consumers. Due to this popularity, Scotch is
the most frequently sold and analyzed whisky type. The aim of the conducted

investigations is to determine the chemical composition of this alcoholic beverage. Besides

gaining knowledge, such research allows for comparing whisky with other popular spirits.

This, in turn, allows determining the specific qualities of whisky for which it is

preferentially chosen by consumers. Due to significant diversity of brands, resulting from

the type and quality of raw materials, production location and production type, scientists

often compare certain types of whisky. The conducted studies also aim at relative quality

comparisons and the determination of features that are characteristic for a given product.

Moreover, whisky is analyzed in order to authenticate it. Because many whisky brands of

different quality are present on the market the occurrence of falsified products, made from

substandard raw materials or by cheaper methods, is frequent. Another issue is aging of

whisky. Older whisky has its own distinctly different taste which translates into different,

usually higher price. Therefore the confirmation of whisky age is of utmost importance.

Among the whisky types, Scotch whisky is falsified most often. Different types of gas

chromatography are preferentially employed to analyze whisky. The more advanced

analysis is conducted by means of two-dimensional gas chromatography, while one-

dimensional gas chromatography is used in the other analysis types. Mass spectrometry,

FID and AED are mostly chosen as detectors. The sample preparation is usually performed

by using SPME technique, with different commercially available fibers. The obtained data

are statistically processed by PCA, PLS regression, ANOVA and DFA methods. Besides

chromatographic analysis, other techniques are also used such as, liquid chromatography,

spectroscopy, electronic nose, and spectrometry. The presently applied methods allowed a

relatively good determination of whisky composition as well as distinguishing whisky from

other spirits and falsified whisky. Thanks to the development of analytical techniques, the

acquisition of other interesting information about spirit-based beverages has become

possible. Despite the fact that whisky

types have been so far researched in detail, the development of chromatographic techniques

coupled with detectors may allow for even more detailed determination of whisky

composition, while the application of analytical devices such as the electronic nose and the

electronic tongue will enable rapid identification of these spirits. Information about markers

characteristic for raw materials and geographic localities of produced whisky are still

lacking. Based on the information reviewed in this paper, the methods described above

have proved to be suitable for analyzing whisky. However, there are still undiscovered

areas related to spirit- based beverages which, when properly researched, would improve

the quality of the produced goods.

Table 1. Examples of analysis of

whisky "Acknowledgments

The authors acknowledge the financial support for this study by the Grant No.

2012/05/B/ST4/01984 from National Science Centre of Poland."

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Table 1. Examples of analysis of whisky

Sample Object of study Apparatus Lit.

American bourbon detection of 23 active aroma substances HRGC-O 9

American bourbon quantitative analysis of 31 compounds TD-HRGC-MS 10

Malt whisky identify green note compounds in malt whisky MDGC-MS-O 11

Scotch and Irish quantitative analysis of the selected compounds GC-MS, SPME 6

whisky

Scotch whisky analysis of ethyl esters GC-GC-MS, SPE 12

Whisky bought in monitoring the contents of 12 selected haloanizoles SPME-GC-AED 14

local market in

Spain

Whisky from 9 analysis of phenols GC-MS 15

countries

Malt whisky from analysis of γ-decalaktone and γ-dodecalactone GC-MS, GC-O 16

Scotland

whisky analysis of ethyl carbamate GC/MS-MS 17

Scotch whisky analysis of ethyl carbamate GC-MS 18

whisky analysis of methanol e-nose 19

whisky analysis of zinc, lead and copper ions ASV, AAS 25

whisky comparison of cachaça, whisky, rum, vodka, gin, GCxGC-TOFMS 26

 tequila and selected liqueurs

Scotch whisky comparison of whisky and cognac GC-MS 29

whisky distinguishing the types of alcoholic beverages e-nose 27

Whisky from distinguish among the whisky samples with regard GC-FID, UV-Vis 30

Canada, Finland, to the country of their origin

Ireland, Scotland

Scotch and Irish distinguish among Scotch and Irish whisky and GC-MS 31,

whisky and bourbon bourbon 34

blended and comparison of whisky and brandy GC-FID 40

malt whisky,

bourbon,

Canadian and

Danish whisky
Scotch whisky distinguishing among various whisky types, i.e. optical 37

blended from single malt spectroscopy

Scotch whisky distinguish among Scottish whiskies of different sensory 42

quality evaluation

Scotch whisky distinguishing among blended whiskies of different SPME-HRGC- 45

quality MS

Black Label, distinguish among specific whisky brands GC-MS, SPME 41

Ballantine's and

West Highlands

Scotch whisky samples differing with regard to brand, age and NIRS 50

barrel type

Blended, malt and determine the region of sample origin and sample AAS 39

grain whisky type

Scotch whisky distinguishing among the analyzed samples, and GC-C-IRMS 46

finding the samples of falsified spirits

 Scotch whisky authentication of Scottish whisky GC-MS 47,

48

Scotch whisky authentication of Scottish whisky UV-Vis 49

Scotch whisky detection of falsified scotch whisky mid-infrared 52

spectrometry

Scotch whisky determining the origin of whisky TC/EA-IRMS 53

Scotch whisky authentication of Scottish whisky FT-ICR MS 54

Scotch whisky authentication of Scottish whisky Capillary 55

electrophoresis

Scotch, American distinguishing among Sottish, American and EI-MS 56

and falsified Brazilian whiskies.

Brazilian whisky

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