Special Issue Paper

Received: 27 February 2012,

Revised: 25 April 2012,

Accepted: 4 May 2012

Published online in Wiley Online Library: 4 June 2012

(wileyonlinelibrary.com) DOI 10.1002/ffj.3105

Characterization of the aromatic prole of the

Quebranta variety of Peruvian pisco by gas
chromatographyolfactometry and chemical
analysis
Juan Cacho,a Laura Culler,a* Liliana Moncayo,a Juan Carlos Palmab and
Vicente Ferreiraa
ABSTRACT: Twenty-one commercial pisco samples made with Quebranta grapes from four different geographical areas in
Peru have been evaluated by gas chromatographyolfactometry (GC-O) and chemical quantitative analysis. The GC-O study
revealed that the Peruvian pisco from the Quebranta grape variety has a relatively simple aroma prole formed by 22 odorants, all of which could be identied. Most of the odorants are fermentation related, while guaiacol, b-damascenone, geraniol
and linalool come from the grape. The chemical analysis of the volatiles of these samples has shown a volatile prole quite
typical of a wine distillate, with not very high but perceptible levels of linalool and b-damascenone (up to 46 mg/l). Some of
the samples contained also very high levels of b-phenylethyl acetate and b-phenylethanol (up to 13 mg/l and 72 mg/l,
respectively), which arises as key aroma compounds potentially responsible for deep sensory differences between samples.
In fact, the differential sensory character of piscos from the Moquegua region can be explained by the lowest levels of
b-phenylethyl acetate, b-phenylethanol, b-damascenone and linalool and also by the highest level of ethyl acetate. In general, differences linked to the geographical area are not very big, although results suggest that the difference could be
enough for classication. Copyright 2012 John Wiley & Sons, Ltd.
Keywords: Quebranta; Peruvian Pisco; aroma; olfactometry; quantitative analysis

Introduction

322

Pisco is a common beverage, originating in some South American

countries (such as Peru and Chile), which is obtained by distillation of wine made from different varieties of grapes. It is considered a high-quality product that is of economical importance.
Its fruity aroma distinguishes this beverage from other young
distillates. Therefore, avour and aroma of pisco are dened with
fruity and owery descriptors, whose origin could be explained
by the variety of grapes used and also by the presence of some
compounds formed during the fermentation and distillation
process.[1]
While the Chilean pisco was obtained mainly from Muscat
grapes, pisco produced in Peru is also obtained from other grape
varieties. It is possible to distinguish between the group of
aromatic grapes (Albilla, Italia, Moscatel and Torontel) and the
non-aromatic grapes (Mollar, Negra Criolla, Quebranta and
Uvina). The most representative varieties of Peruvian pisco are
Italia and Quebranta. It should be noted that Quebranta is also
the most used variety for obtaining non-aromatic pure pisco.
All of these different varieties of grape are particularly appropriate in different valleys, depending on the quality of soil and
climate characteristics. The region of Ica seems to be an
adequate area for all varieties in general, being the region with
the highest production of grapes, due to the benecial
agronomic conditions, the use of new technology and optimum
climatic conditions, dened as semi-warm and with low rainfall.

Flavour Fragr. J. 2012, 27, 322333

Moreover, heat stroke is higher than in other regions, which is

advantageous to ensure high reducing sugar levels in grapes
(which can reach 16 ).
Nowadays, and in spite of the fact that this distillate has been
produced since at least the 16th century,[2] very few studies have
been published about its characteristic aroma composition and,
in fact, all of them deal with pisco from Chile and not from
Peru.[36] In 1990 Herraiz et al.[5] presented an application of a
multi-dimensional gas chromatography method for characterizing the volatile composition of Chilean Pisco. On the other hand,
Agosin et al.[3] provided a quantication of the most relevant
terpenes and other aromatic compounds present in the most

* Correspondence to: Laura Culler, Laboratory for Aroma Analysis and Enology, Aragn Institute of Engineering Research (I3A), Department of Analytical
Chemistry, Faculty of Sciences, University of Zaragoza, Zaragoza 50009, Spain.
E-mail: lcullere@unizar.es

This article is published in Flavour and Fragrance Journal as Part I of Special

Issue: 13th Weurman Flavour Research Symposium, Zaragoza, Spain, 27th 30th
September 2011, edited by Vicente Ferreira (University of Zaragoza).
a

Laboratory for Aroma Analysis and Enology, Aragn Institute of Engineering Research (I3A), Department of Analytical Chemistry, Faculty of Sciences,
University of Zaragoza, Zaragoza 50009, Spain

University la Molina, Lima, Peru

Copyright 2012 John Wiley & Sons, Ltd.

Aromatic prole of Peruvian Quebranta piscos

signicant varieties to the industry (Moscatel de Alejandra,
Moscatel Rosada, Moscatel de Austria y Torontel). Finally, another
two studies were carried out in order to provide standardized
terminology to describe sensory differences among the wide
range of piscos.[4,6] In both papers, a selection of relevant sets of
attributes has been chosen by well-trained subjects. However,
and to the best of our knowledge, the systematic screening of
pisco odorants by gas chromatographyolfactometry (GC-O)
has not been carried out.
The main aim of this study is to characterize the odorant
prole of Quebranta Piscos belonging to different regions of
Peru (Lima, Ica, Arequipa and Moquegua), using GC-O, GC with
ame ionization detection (FID) and GC with mass spectrometry
detection (GC-MS).

Pisco extract was obtained by a dynamic headspace sampling technique (DHS-SPE) used previously in our laboratory.[7]
A standard solid phase extraction (SPE) cartridge (0.8 cm
internal diameter, 3 ml internal volume) lled with 400 mg of
LiChrolut EN resins was rst washed with 20 ml of dichloromethane and then dried by allowing air to pass through
(negative pressure of 0.6 bar, 10 min). The cartridge was
placed on the top of a ask containing 80 ml of pisco at room
temperature (approximately 21 C). A stream of nitrogen
(500 ml/min) was applied onto the surface of the liquid, purging the volatile compounds of the headspace. The volatile
pisco components released were trapped in the cartridge containing the sorbent.
Extraction time optimization

Material and Methods

Pisco Samples
Twenty-one Peruvian pisco elaborated with Quebranta grapes
were studied in this work. Five of them were from Arequipa, six
from Ica, six from Lima and the other four from Moquegua. Table 1
provides detailed information about all these samples analysed.

Reagents and Standards

Dichloromethane and methanol of LiChrosolv quality were from
Merck (Darmstadt, Germany), absolute ethanol was from
Panreac (Barcelona, Spain). Pure water was obtained from a
Milli-Q purication system (Millipore, Bedford, MA, USA). Semiautomated solid-phase extraction (SPE) was carried out with a
VAC ELUT 20 station from Varian (Walnut Creek, CA, USA). The
LiChrolut EN resins and polypropylene cartridges were obtained
from Merck.
The chemical standards used for identications were supplied
by Aldrich (Steinheim, Germany), Fluka (Buchs, Switzerland),
Poly-Science (Niles, Illinois, USA), Lancaster (Strasbourg, France),
Alfa Aesar (Karlsruhe, Germany). An alkane solution (C8C28),
20 mg/l in dichloromethane, was employed to calculate the
linear retention index of each analyte.

Gas ChromatographyOlfactometry
Extract preparation
One representative sample of this variety of pisco (Quebranta)
was prepared in order to characterize, from an olfactometric
point of view, its aromatic prole. For this, equal volumes of
piscos from the different regions were mixed.

It has been determined the optimal purge time to extract the

volatile compounds present in pisco samples in the DHS-SPE
system. The high level of alcohol that this distillate contains
(3848%) must be taken into account. Therefore, it was necessary to evaluate how it affects the content of alcohol in the
method of extraction and retention of the volatile compounds
in our purge and trap system. In the case of wine samples
(1214% alcohol), this time was established as 100 min.[810]
The following experiment (see Figure 1) was carried out in
order to avoid the loss of aromatic compounds because of
the saturation of the resins, provoked by this high level of
alcohol. A second SPE cartridge of 200 mg of LiChrolut EN
resins was placed after the rst cartridge, used as a trap, and
replaced every 10 min. The third and fourth cartridges were
replaced after 15 min, and the fth and sixth after 25 min.
Volatile compounds trapped in all these cartridges were eluted
by 1.6 ml of ethanol, and the 400 mg orginal cartridge (used as
trap) was eluted with 3.2 ml of ethanol. The next step was to
dilute all these samples with distilled water to reach 12%
ethanol. A sensory evaluation was carried out with the help
of a panel composed of eight trained judges in order to evaluate the percentage of aromatic compounds lost depending on
the extraction time. All of these diluted extracts, including the
reference sample from the trap cartridge, were served in
coded, tulip-shaped wine glasses covered by glass Petri dishes
(20 ml at 21 C). Samples were presented in random order.
Judges were asked to evaluate ortho-nasally the similarity
between the intensity of each of these samples and the
reference sample. The higher the score, the greater similarity
exists between samples. This similarity indicates a high loss
of aromatic compounds because they have not been retained
in the trap cartridge.
As a result of this experiment, a time of 20 min was established
as optimum. Therefore, after this time, the cartridge was removed

Table 1. Quebranta pisco samples analysed in this study according to their origin
Lima (n = 6)

Flavour Fragr. J. 2012, 27, 322333

Arequipa (n = 5)

Clsico
Grimaldi
Bellavista
Bodega Yanquiza
Don Fede 2009
Payet

Majes Tradicin
Cepas de Loro 2007
La Hacienda del Abuelo
Cepas de Loro 2008
Mi dolo

Copyright 2012 John Wiley & Sons, Ltd.

Moquegua (n = 4)
Cutip
Bondi 2008
OMO Zapata
Jimnez

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323

El Sarcay
Don Amadeo
Andrs Arias
UNA 2005
UNA 2008
Gran Cruz

Ica (n = 6)

J. Cacho et al.

Figure 1. Scheme of the experiment designed in order to avoid the loss of aromatic compounds because of the saturation of the resins, provoked by
this high level of alcohol. The extracts obtained were diluted with distilled water to reach 12% of ethanol and were evaluated by a sensory panel

and dried by allowing nitrogen to pass through to avoid possible

condensation of water. Then, analytes are eluted with 3.2 ml of
dichloromethane with 5% methanol. After this operation, the
extract was concentrated under a stream of pure nitrogen to a
nal volume of 200 ml.

as a percentage of total number of judges and I(%) is the average

intensity expressed as percentage of the maximum intensity.

Gas chromatographyolfactometry analysis

This analysis was carried out following the principle proposed by

Lpez-Vazquez et al.[14] This methodology consists of the direct
injection of the pure distillate into a gas chromatograph system,
after addition of an internal standard. The calibration of the
method was developed using dilute solutions of pure standards
(see Table 2). Then, 1.6 ml of Pisco containing 20 ml of internal
standards solution (4-methyl-2-pentanol and 4-decanol,
2000 mg/l) was analysed by GC with FID detection under the
following conditions. A gas chromatograph STAR 3400 CX series
from Varian equipped with a FID was used. The column was a
DB-Wax from Varian, 50 m  0.32 mm i.d., with 0.2 mm lm
thickness. The carrier was hydrogen at 4 ml/min. One microlitre
of the pisco sample was injected in split mode, split ratio 1/10.
Injector and detector were both kept at 220 C. The temperature
program was as follows: 40 C for 3 min, then raised at 6 C/min
to 75 C, and at 9 C/min to 220 C, and nally was held at 220 C
for 10 min.

324

All snifng experiments were carried out in a Trace gas chromatograph from TermoQuest, equipped with ame ionization
detector (FID) and a snifng port (ODO-1 from SGE) connected
by a ow splitter to the column exit. The columns used were a
DB-WAX from J&W (Folsom, CA, USA), 30 m  0.32 mm ID,
0.5 mm lm thickness and a VF-5ms from Varian (30 m  0.25 mm
ID, 0.25 mm lm thickness). A constant pressure of 52 kPa was
maintained throughout the analysis time. The carrier gas was
hydrogen. One microlitre was injected in splitless mode for
1 min splitless time. Injector and detector were both kept at
250 C. The temperature program was 40 C for 5 min, then
increased by 4 C/min to 100 C followed by 6 C/min to 220 C,
and nally kept at 220 C for 20 min. To prevent condensation
of high-boiling compounds on the snifng port, the port was
heated sequentially with a laboratory-made rheostat.
The olfactometric strategy carried out in this study combines
measurements of intensity and of frequency of detection and
has been widely used in previous papers published by members
of our laboratory.[912]
For this GC-O study, snifngs were carried out by a panel
composed of six expert judges belonging to our laboratory. The
extracts, once concentrated to 200 ml, were smelt once by each
panellist. Snifng time was approximately 40 min, and each judge
took part in one session per day. Panellists were asked to score the
intensity of each aromatic stimulus using a four-point scale
(0 = not detected, 1 = weak, 2 = clear but no intense note,
3 = intense note). The data processed were a mixture of the intensity and the frequency of detection of an odorant. This parameter
is labelled modied frequency (MF) and is calculated with the
formula proposed by Dravnieks:[13] MF(%) = [F(%)  I(%)], where
F(%) is the detection frequency of an aromatic attribute expressed

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Chemical Quantitative Analyses by Direct Injection of the

Distillate into a Gas Chromatograph

Chemical Quantitative Analyses by Solid Phase Extraction

Followed by Injection into a Gas Chromatograph
This analysis was carried out using the method proposed and
validated by Lpez et al.[15] with some modications. In accordance with this method, 15 ml of pisco were diluted up to
50 ml with Milli-Q water in order to obtain a 12% (v/v) ethanol.
A volume of 26 ml of a surrogate standards solution (3-octanone
and b-damascone of 200 mg/l) were added to the sample
and then passed through a LiChrolut EN cartridge at about
2 ml/min. The sorbent was dried by allowing air to pass through
it ( 0.6 bar, 10 min). Analytes were recovered by elution
with 1.6 ml of dichloromethane. An internal standard solution
(4-hydroxy-4-methyl-2-pentanone and 2-octanol, 200 mg/l) was

Copyright 2012 John Wiley & Sons, Ltd.

Flavour Fragr. J. 2012, 27, 322333

Aromatic prole of Peruvian Quebranta piscos

Table 2. Linearity data of the methodology based on the direct injection of the pisco samples in a gas chromatograph (GC-FID)
Compound
a

Acetaldehyde
Isobutanala
Methyl acetatea
Ethyl acetatea
Propanola
Isobutanola
1-Butanola
2-Methyl-1-butanola
3-Methyl-1-butanola
3-Hydroxy-2-butanonea
Ethyl lactateb
1-Hexanolb
Ethyl octanoateb
Furfuralb
Acetic acidb
2,3-Butanediolb
Diethyl succinateb
b-Phenylethanolb

Slope

Intercept

0.0193
0.0350
0.0252
0.0344
0.0526
0.0643
0.0536
0.0838
0.0698
0.049
0.0323
0.0493
0.0528
0.0289
0.0183
0.0308
0.0836
0.0596

0.1032
0.0434
0.0418
0.6700
0.9157
1.1783
0.1217
0.5843
1.2302
0.4688
0.2798
0.1479
0.0038
0.0090
0.1275
0.0115
0.0338
0.2279

r2

Calibrated range (mg/l)

LD* (mg/l)

RSD** (%)

0.999
0.997
0.996
0.994
0.994
0.994
0.992
0.996
0.994
0.994
0.996
0.992
0.999
0.996
0.995
0.993
0.999
0.992

0.14850
0.1077
0.03793
0.0467100
0.0035240
0.0151367
0.005298
0.019310
0.0141287
0.01470
0.027309
0.01120
0.003620
0.01120
0.0811688
0.027200
0.003142
0.0054237

0.14
0.10
0.037
0.046
0.0035
0.015
0.0052
0.019
0.014
0.014
0.027
0.011
0.0036
0.011
0.081
0.027
0.0031
0.0054

1.4
4.6
4.9
1.8
3.3
4.8
1.2
2.6
1.5
5.4
3.0
1.7
5.2
2.1
2.7
2.4
4.5
2.1

*LD: Limit of detection was dened as the concentration which gives a signal to noise ratio of 3. For its calculation the s/n ratio of
samples, which contain very low amounts were used.
4-Methyl-2-pentanol (a) and 4-decanol (b) were used as internal standards.
** Relative standard deviation was calculated by mean of 16 determinations (4 days  4 replicates/day) of three different pisco samples.

added to the eluted sample. The extract was then analysed by

GC with ion trap MS detection under the conditions described
by Lpez et al.[15] There are 23 compounds which were not

quantied in the previous paper, considered as the reference.[15]

Therefore, Table 3 provides calibration information about this
group of compounds.

Table 3. Calibration data of 23 compounds, which are analysed by a solid phase extraction followed by injection in a gas
chromatograph and were not quantied in a previous paper[15]
Compound

Slope

43
71
57
RIC
88
67
67
59
59
93 + 121 + 136
105
95
11 + 120
157 + 201
69 + 93
69
123
108
108
85
99
69
181.0 + 182.0

0.0011
0.00312
0.0005
0.0187
0.00312
0.000937
0.000864
0.000437
0.000443
0.00118
0.00184
0.00125
0.0007
0.00153
0.00625
0.00038
0.0002
0.00052
0.00083
0.00154
0.000795
0.000287
0.00134

Flavour Fragr. J. 2012, 27, 322333

Intercept
0.0447
0.0096
0.0005
0.0061
0.0361
0.0014
0.0015
3.1E 05
2.5E 05
1.5E 06
0.0061
0.0003
0.0011
0.011
0.0002
8.3E 06
0.0039
9.3E 05
9.00E 06
0.0017
3E 05
0.00022
0.0237

r2

Calibrated range (mg/l)

LD (mg/l)

0.993
0.999
0.998
0.988
0.997
0.987
0.999
0.999
0.999
0.999
0.999
0.992
0,999
0.992
0.995
0.999
0,999
0.998
0.996
0.993
0.995
0.999
0.995

1.301372
11.29395
3.39784
0.442906
0.029395
0.31506
6.0310000
0.205000
0.105000
0.101000
0.14137
0.6024
0.30997
7.3010000
0.30147
0.765000
1.0711962
0.975000
0.083.80
0.0772.5
0.1418.3
3.225000
0.02522

1.30
11.2
3.39
0.44
0.02
0.31
6.03
0.20
0.10
0.10
0.14
0.60
0.30
7.30
0.30
0.76
1.07
0.97
0.08
0.07
0.14
3.22
0.02

Copyright 2012 John Wiley & Sons, Ltd.

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325

Isobutyl acetate
Ethyl butyrate
Ethyl isovalerate
Isoamyl acetate
Ethyl hexanoate
trans-Limonene oxide
cis-3-Hexenol
cis-Linalool oxide
trans-Linalool oxide
a-Terpinolene
Benzaldehyde
Ethyl furoate
Phenylacetaldehyde
Ethyl decanoate
Neryl acetate
Nerol
Geraniol
Benzyl alcohol
m-Cresol
g-Decalactone
d-Decalactone
Farnesol
Syringaldehyde

m/z

J. Cacho et al.
100

The sensory panel was composed of nine females and one

male, 2435 years of age, all of whom belonged to the laboratory staff and with a long experience in sensory analysis.
Four specic 1 h training sessions were carried out. In the rst
one, judges generated descriptive terms to dene the pisco
samples of this study, considering the pisco wheel developed
by Bordeu et al.[4] These authors identied the 20 descriptors
most frequently used by their trained panel. In sessions 2 and
3, different aroma standards were presented and discussed
by the panel. From these discussions, nine aroma attributes
were chosen as the most appropriate to describe our pisco
samples. This group of descriptors included: fresh fruit, raisins, oral, cut grass, woody, sweet, oxidized, spicy and nuts.
In training sessions four, panellists scored the intensity of
each attribute using a seven-point scale (0 = not detected),
1 = weak, hardly recognizable note, 2 = clear but no intense
note, 3 = intense note); half values were allowed. After the
training period, Quebranta samples from the different regions
were evaluated. The data were processed to calculate the
modied frequency parameter proposed by Dravnieks,[13]
as in the case of the olfactometry data.
Statistical Analysis
For the data obtained from the chemical quantitative data, a
one-factor (origin) analysis of variance, ANOVA test, was carried
out to look for discriminant odorants. In the case of data
obtained from sensorial descriptive another one-factor (origin)
analysis, ANOVA, also was carried out to look for discriminant
aromatic descriptors. All these analyses were performed using
SPSS software (version 15.0) from SPSS Inc. (Chicago, IL, USA).
Furthermore, principal component analysis was carried out
using Unscramble vs. 9.7 from Camo (Oslo, Norway).

Results and Discussion

Gas ChromatographyOlfactometry

Aromatic similarity (%)

Sensory Descriptive Analysis

90
80
70

61%

65%

60
50

50%

48%

35

50

40
30
20

17%

18%

10

20

10
0
75

100

Time (min)
Figure 2. Optimization of the extraction time depending on the aromatic
similarity between the extract obtained from the second cartridge and the
original extract

indicating that the breakthrough of the trap had occurred

between 20 and 35 min.
Olfactometric prole
The GC-O study was carried out in a single sample made by
proportional mixing of all the exemplars of Peruvian Quebranta
piscos, as described in the Material and Methods section. Results
of the GC-O study are given in Table 4, and are ranked according
to their sensory scores. All odorants could be identied, although
in the cases of 2-methyl-3-furanthiol and sotolon, a specic MS
of the compound in the GC-O extract could not be obtained.
The olfactometric prole is typical of a naturally fermented alcoholic beverage, with 2,3-butanedione, isoamyl alcohol and ethyl
2- and 3-methylbutyrates as most important odorants. All the
components are well known wine components and most of them
are by-products of yeast fermentation. An exception to this are
guaiacol, b-damascenone, geraniol and linalool, which are most
likely grape components, and sotolon and phenylacetaldehyde
that are the most likely result of oxidation of the corresponding
amino acid precursors during the distillation.[16,17]

Purge time optimization

326

A purge and trap system specically designed for providing

vapour compositions as close as possible to those observed
during ortho-nasal olfaction was used. As the system was originally designed for working with wines with alcoholic degrees
not in excess of 16% (v/v), a study was carried out in order to
determine when the higher alcohol levels of pisco samples
would cause breakthrough of the trap. With this purpose the
efuent of the trap was trapped again in a second trap set in
tandem after the rst. This second trap was replaced by a new
one after different purging times (see methods), eluted with
ethanol, diluted with mineral water, and this diluted extract
evaluated by sensory analysis in order to assess its similarity to
the pisco. Results of the analysis are given in Figure 2. As can
be seen, the extracts from the two rst cartridges containing
the volatile molecules coming out the rst trap after 10 and
1020 min of purging, were completely different to the pisco
from a sensory point of view. In fact, these extracts were considered to be not signicantly different to diluted ethanol (data
not shown), indicating that the trapping in the rst 20 min is
complete. However, the extract taken from the third cartridge
was found to be signicantly more similar to the pisco sample,

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Chemical Aroma Composition

Two different analytical methods were used in order to characterize the volatile chemical composition of the Quebranta pisco
samples. Eighteen major volatile compounds were determined
by direct injection of the pisco samples in a GC-FID system.
Analytical details of this procedure are given in Table 2 and
quantitative results of the samples, grouped by geographical
origin, are given in Table 5. Another 41 different compounds
were determined by the GC-MS analysis of extracts obtained
by solid phase extraction from diluted pisco, and results are
given in Table 6. Three relevant odorants reported in Table 4
could not be quantied: 2,3-butanedione because it could not
be separated from ethanol in the direct injection method, and
sotolon and 2-methyl-3-furanthiol because their concentrations were below the method detection limits. Compounds
related to wood-ageing, such as cis-whiskylactone (LD = 0.5 mg/l),
d-decalactone (LD = 0.1 mg/l), methyl vanillate (LD = 0.04 mg/l),
acetovanillone (LD = 0.03 mg/l) and syringaldehyde (LD = 0.02 mg/l)
were also not detected, just conrming that these samples did
not have any contact with wood along their production.

Copyright 2012 John Wiley & Sons, Ltd.

Flavour Fragr. J. 2012, 27, 322333

Aromatic prole of Peruvian Quebranta piscos

Table 4. Odorants found by GC-O in the representative sample of Quebranta pisco: gas chromatography retention data, olfactory
description, chemical identity and modied frequency percentage, MF (%), are given for each compound
LRI

DB-WAX

962
1223
1078
1063
1316
2226
1680
1874
1039
1015
1242
1457
1839
1935
1858
1129
1381
1551
1660
1641
2259
1829

LRI

VF-5ms

600
719
856
846
890
1114
898
1137
800
771
999
600
1392
1108
1350
860
939
1099
1045
820
1328
1258

Odour descriptor
Butter, cream
Fusel
Fruity, anise
Fruity, anise
Onion, meaty
Curry, licorice
Cheese
Phenolic, medicinal
Fruity
Sweet, solvent
Anise
Vinegar
Baked apple
Roses
Floral, metallic
Banana
Grass
Floral
Floral
Cheese
Phenolic
Floral, roses

Identity

MF (%)
a

2,3-Butanedione
Isoamyl alcohola
Ethyl 3-metylbutyratea
Ethyl 2-metylbutyratea
2-Methyl-3-furanthiolb
Sotolonb
3-Methylbutyric acida
Guaiacola
Ethyl Butyratea
Isobutyl acetatea
Ethyl hexanoatea
Acetic acida
b-Damascenonea
b-Phenylethanola
Geraniola
Isoamyl acetatea
1-Hexanola
Linaloola
Phenylacetaldehydeb
Butyric acida
4-Vinylguaiacola
b-Phenylethyl acetatea

87
85
78
63
63
63
59
59
57
57
55
47
36
35
35
33
26
22
22
22
22
20

a
Identication based on the coincidence of gas chromatographic retention indices in DB-WAX and VF-5ms columns, olfactory
description and mass spectrum.
b
Identication based on the coincidence of gas chromatographic retention indices in DB-WAX and VF-5ms columns, olfactory
description but these compound did not produce any clear signal in the mass spectrometer.

Flavour Fragr. J. 2012, 27, 322333

although far below the amounts that some Muscat grapes can
contain.[3,5] b-Damascenone, with a typical baked-apple odour,
and known contributor to wine fruity and raisin character,[21]
reaches high levels, far higher than those found even in wines
made with sun-dried grapes.[8] The maximum value of 46 mg/l
was found in one of the Arequipa samples, but average values
are in all cases around or above 20 mg/l. Anyway, these levels do
not differ from the mean concentrations found in German and
French grape brandies (15 and 35 mg/l, respectively).[22] On the
other hand, Cognac brandies had considerably higher concentrations of these compounds (102257 mg/l), which could be
attributed to the distillation method employed for Cognac production.[22] Recently, Zhao et al.[23] have detected a very high level of
b-damascenone in one sample of brandy (40 mg/l). Another
interesting nding concerns the high levels found for the rosesmelling ester b-phenylethyl acetate. Three of the samples from
Lima were found to contain more than 7 mg/l (one of them even
reaching up to 13 mg/l), but most samples contained levels below
5 mg/l. It should be considered that, in this case, differences
between the most diluted (85.5 mg/l) and the most concentrated
(13117 mg/l) samples are more than two orders of magnitude,
which suggests that this compound will be responsible for strong
aroma differences between these Quebranta pisco samples. In
fact, this variety of pisco contains higher levels of this acetate than
other wine distillates. Herraiz et al.[5] determined levels between
100 and 5000 mg/l in Chilean pisco made from Muscat grapes,
Lpez-Vazquez et al.[14] reported lower levels for b-phenylethyl
acetate in orujo samples (between 50 and 250 mg/l) and other
authors showed concentrations between 200 and 1600 mg/l in

Copyright 2012 John Wiley & Sons, Ltd.

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327

Quantitative results are in accordance with the nature of a

wine distillate. Major compounds are major fermentation metabolites, such as ethyl acetate, 3-methyl-1-butanol, 2-methyl-1butanol, acetic acid and isobutanol. Leaving aside these major
compounds found at typical levels in distillates, some results in
Table 5 and Table 6 deserve particular comment. Comparing
the volatile composition to pisco with other wine distillates as
orujo,[14] grappa[18] or different brandies,[19,20] it can be concluded that, in general, the levels of the major compounds in
all these beverages are very similar. However, some differences
must be noted regarding their composition. Therefore, this
variety of pisco is highlighted due to its highest levels of
b-phenylethanol (1171.5 mg/l), and b-phenylethyl acetate
(0.08513.1 mg/l). Another characteristic of Quebranta pisco is
the small amounts of some ethyl esters (0.0500.200 mg/l
for ethyl hexanoate, 0.22.1 mg/l for ethyl octanoate and
0.13 mg/l for ethyl decanoate) in comparison to the levels
found in other distillates. For example, grappa samples and different brandies have shown levels of ethyl hexanoate between
3 and 15 mg/l and levels of ethyl decanoate up to more than
40 mg/l. Referring to higher alcohols, as it is the case of propanol,
isobutanol and 2-methylbutanol, it can be concluded that some
brandies are characterized by higher levels of these compounds
than in Quebranta pisco.
In spite of the fact that Quebranta grapes are considered
a non-aromatic grape variety, all Quebranta piscos analysed
contained relatively high amounts of linalool, cis-linalool
oxide, trans-linalool oxide and a-terpineol, well above the
corresponding odour thresholds in hydroalcoholic solutions,

328

wileyonlinelibrary.com/journal/ffj

Copyright 2012 John Wiley & Sons, Ltd.

18.4
1.5
2.6
76.9
14.9
92.4
2.4
60.0
302
9.9
12.4
1.7
0.4
0.9
61.9
14.4
1.1
11.7

Min

59.2
2.2
4.2
133
79.2
173
3.6
140
706
10.7
35.9
2.6
2.1
2.1
186
39.4
4.2
48.3

Max
29.8
1.7
3.4ab
76.5
39.4
127
2.9
97.9
475
10.4
23.2
2.1
1.2
1.4b
99.4
25.2
2.7a
26.5

Av

Arequipa (n = 5)

16.7
0.3
0.7
35.2
25.3
38.3
0.4
33.0
162
0.3
9.2
0.3
0.7
0.5
54.6
11.0
1.3
14.1

SD
21.0
1.5
2.9
33.1
19.7
89.4
2.1
71.7
328
9.8
11.2
1.7
0.5
1.3
15.6
11.7
0.6
16.6

Min
69.0
2.4
5.4
116
52.2
206
8.2
121
598
12.3
41.8
3.9
1.3
5.1
124
32.2
2.9
48.8

Max
37.3
2.0
4.2a
63.8
34.5
136
4.2
104
497
11.2
24.1
2.4
0.8
3.5a
84.1
22.1
2.1a
37.5

Av

Ica (n = 6)

17.3
0.3
1.0
29.9
13.3
42.5
2.5
20.7
93.4
0.9
11.8
0.8
0.4
1.4
37.2
6.6
0.8
13.2

SD
22.8
1.3
3.3
46.2
20.2
89.3
2.1
75.0
311
10.3
10.3
1.5
0.2
1.8
47.6
16.3
0.5
23.0

Min
69.9
2.6
4.3
207
68.1
208
5.5
151
548
14.9
27.2
3.9
0.8
5.2
180
40.4
1.2
71.5

Max
39.8
1.9
3.7a
31.6
46.3
127
3.3
105
391
11.7
15.3
2.1
0.5
3.3a
117
30.1
0.8b
39.2

Av

Lima (n = 6)

18.0
0.4
0.3
58.7
17.9
42.4
1.2
30.2
120
1.8
6.2
0.9
0.3
1.4
46.7
10.5
0.3
19.4

SD
14.0
1.4
2.1
51.5
34.8
84.6
2.5
70.2
323
9.8
14.7
2.4
0.3
0.5
15.8
10.9
1.9
10.9

Min

31.7
1.7
3.2
200
82.9
172
4.3
107
448
10.3
60.2
3.8
0.8
2.1
220
24.8
3.9
23.2

Max

21.3
1.5
2.7b
103
48.8
128
3.0
89.4
396
10.0
32.1
3.0
0.6
1.2b
102
17.2
2.6a
18.3

Av

Moquegua (n = 4)

7.4
0.2
0.5
67.3
22.9
36.4
0.8
15.8
54.6
0.3
19.6
0.6
0.2
0.8
85.9
6.3
0.9
5.4

SD

Compounds that differed signicantly (> 95%) in an ANOVA analyses are marked with an asterisk (*).
* Statistically signicant differences measured by ANOVA at p < 0.05 according to region of origin.
Duncans test results are shown with different letters: a.b.c.
Av: Average concentration, min: minimum concentration; Max: maximum concentration, and SD: standard deviation.
The identication of all these compounds based on the coincidence of gas chromatographic retention time in DB-WAX column with those of the pure compounds.

Acetaldehyde
Isobutanal
Methyl acetate
Ethyl acetate
Propanol
Isobutanol
1-Butanol
2-Methyl-1-butanol
3-Methyl-1-butanol
3-Hydroxy-2-butanone
Ethyl lactate
1-Hexanol
Ethyl octanoate
Furfural
Acetic acid
2,3-Butanediol
Diethyl succinate
b-Phenylethanol

Compound

ANOVA

Table 5. Compounds analysed by direct injection of the distillate in a GC-FID: Average concentration levels (in mg/l) and standard deviation found in different Quebranta samples
belonging to different regions (Arequipa, Ica, Lima and Moquegua)

J. Cacho et al.

Flavour Fragr. J. 2012, 27, 322333

329

Flavour Fragr. J. 2012, 27, 322333

Isobutyl acetate
Ethyl butyrate
Butyl acetate
Ethyl 2-methylbutyrate
Ethyl isovalerate
Isoamyl acetate
Ethyl hexanoate
trans-Limonene oxide
cis-3-Hexenol
cis-Linalool oxide
trans-Linalool oxide
a-Terpinolene
Benzaldehyde
Linalool
Ethyl furoate
Phenylacetaldehyde
Ethyl decanoate
a-Terpineol
Neryl acetate
b-Citronellol
Nerol
b-Damascenone
b-Phenylethyl acetate
Geraniol
Guaiacol
Benzyl alcohol
Ethyl dihydrocinnamate
cis-Whiskylactone

Compound

76.3
61.1

20.1
42.6
77.2
58.9
1.3
50.2
26.4
11.6
1.5
30.9
121
9.1
1.6
566
34.4
1.9
22.7
23.4
9.0
85.5
28.5
<0.1
136
0.6

Min
279
125
<0.8b
135
229
770
192
5.3
89.4
134
99.4
4.3
70.9
614
28.9
6.7
2947
236
3.1
48.5
90.4
46.1
2340
90.8
7.6
947
1.7
<0.5

Max
170
85.6ab

52.8
101
432
117
2.6
68.7
63.1
42.3
3.2
42.5b
271
20.2ab
4.8
1597
100
2.7a
39.7
40.2
26.2
1373b
43.0
3.4c
438
1.1

Av

Arequipa (n = 5)

87.9
24.0

47.2
76.8
296
51.1
1.6
17.5
49.2
38.8
1.1
16.4
195
7.5
2.3
1016
88.5
0.5
11.0
28.2
13.7
1029
25.4
3.3
323
0.5

SD
117
89.3
<0.8
8.9
19.5
176
69.9
1.9
49.8
33.4
22.5
1.5
40.2
99.2
18.2
1.8
660
41.0
2.5
29.6
14.8
6.1
603
24.1
8.5
303
1.1

Min
281
206
5.7
126
252
1594
142
7.8
117
185
119
3.7
102
548
35.7
5.8
1612
211
2.7
62.3
71.1
31.9
5885
82.2
15.2
932
4.0
<0.5

Max
171
147a
2.4b
54.0
102
502
100
4.0
105
82.8
56.9
2.8
74.1a
272
26.1ab
3.8
1099
107
2.6a
43.2
37.2
20.6
2711ab
51.6
12.5a
456
2.2

Av

Ica (n = 6)

61.6
42.4
1.8
39.2
79.1
538
32.2
2.3
47.9
64.2
37.1
0.9
23.1
165
6.6
1.5
397
63.7
0.1
15.0
19.6
10.4
1777
22.2
2.4
240
1.1

SD
106
30.7

10.3
19.0
153
24.9
1.7
54.6
39.1
21.4
2.0
30.5
96.6
15.3
2.4
135
48.4
1.8
27.0
16.6
10.0
1568
22.3
2.6
100
1.2

Min
257
92.9
<0.8b
58.5
95.2
592
95.6
5.0
83.8
106
78.9
7.3
77.1
708
50.9
11.9
1492
203
2.6
131
88.9
39.3
13117
89.0
12.4
767
6.3
<0.5

Max
158
68.8b

28.9
49.5
348
64.8
2.7
67.9
58.7
36.5
3.7
58.2ab
279
32.3a
6.4
688
106
2.2b
54.2
41.2
23.2
6336a
44.6
8.1b
331
2.8

Av

Lima (n = 6)

51.6
27.1

18.0
27.8
194
30.1
1.2
12.3
24.8
22.8
2.0
19.7
247
12.4
3.5
509
69.7
0.3
40.1
28.2
13.3
4989
25.0
3.4
243
2.2

SD
129
65.9
9.9
10.7
20.6
229
65.1
1.2
64.7
19.2
11.9
2.4
23.9
87.6
8.0
3.5
196
26.2
2.0
35.2
28.1
11.7
531
34.0
3.2
299
1.2

Min
286
250
13.3
86.4
177
801
117
2.6
152
51.1
26.5
3.2
49.7
212
24.9
5.7
789
91.6
2.3
51.0
54.2
29.6
1462
49.5
10.4
707
2.2
<0.5

Max

178
134a
11.6a
38.4
75.2
388
101
1.7
119
28.4
16.0
2.8
36.7b
161
14.8b
4.8
553
45.2
2.2b
40.8
39.3
18.2
815b
38.4
5.8bc
510
1.6

Av

Moquegua (n = 4)

72.1
80.4
1.7
33.7
70.8
276
24.2
0.6
37.8
15.1
7.1
0.3
11.2
56.4
7.3
0.9
267
31.1
0.1
7.0
12.1
7.9
435
7.5
3.2
186
0.5

SD

Copyright 2012 John Wiley & Sons, Ltd.

(Continues)

*
*

ANOVA

Table 6. Compounds analysed by SPE and GC-ion trap-MS: average concentration levels (mg/l) and standard deviation found in different Quebranta samples belonging to different
regions (Arequipa, Ica, Lima and Moquegua)

Aromatic prole of Peruvian Quebranta piscos

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Copyright 2012 John Wiley & Sons, Ltd.

2.4
7.0
0.9
1.0

0.6
1.3
2.3

5.2
<0.1
79.1
338
<0.03

0.3

Min
4.7
29.8
8.5
2.2
<0.02
1.9
6.8
23.7
<0.1
49.2
0.3
496
1411
3.1
<0.04
2.4
<0.03
<0.02

Max
3.3
17.4
3.5
1.6b

1.0
2.9
9.9

29.2a
0.1
372
860
1.4

1.2a

Av

Arequipa (n = 5)

1.0
9.5
3.1
0.5

0.5
2.3
8.5

18.0
0.1
168
394
1.2

0.9

SD
4.7
18.1
3.2
2.3
0.1
0.4
2.0
5.2

3.3

242
437
0.5

0.3

Min
6.4
44.2
35.1
5.3
0.8
1.7
6.3
48.6
<0.1
21.0
<0.1
1015
777
2.4
<0.04
2.0
<0.03
<0.02

Max
5.5
29.0
14.4
4.0a
0.3
1.1
3.9
21.1

9.1b

473
552
1.3

1.1a

Av

Ica (n = 6)

0.7
9.1
14.0
1.1
0.3
0.5
1.4
16.9

6.3

281
125
0.7

0.6

SD
2.6
13.5
2.0
1.6
0.1
1.0
1.4
6.3

0.7

313
238
0.2

Min
8.3
49.3
21.7
5.5
0.2
3.8
4.4
62.0
<0.1
7.9
<0.1
702
2012
1.0
<0.04
<0.05b
<0.03
<0.02

Max
5.3
30.1
7.8
3.8a
0.1
2.2
2.7
30.0

4.0b

477
823
0.5

Av

Lima (n = 6)

2.1
13.9
7.8
1.4
0.1
1.2
1.2
20.0

2.7

135
651
0.3

SD
2.8
12.7

1.3
<0.02
1.0
1.1
3.1

2.5

146
215
0.1

Min

10.6
38.1
<0.1
5.1
0.7
2.3
2.9
29.2
<0.1
10.2
<0.1
269
950
0.7
<0.04
<0.05b
<0.03
<0.02

Max

6.8
25.7

2.7ab
0.2
1.6
2.1
12.7

5.7b

200
587
0.5

Av

Moquegua (n = 4)

3.8
12.2

1.8
0.3
0.7
0.8
11.4

3.5

52.9
326
0.3

SD

ANOVA

Compounds differed signicantly (> 95%) in an ANOVA analyses are marked with an asterisk (*).
* Statistically signicant differences measured by ANOVA at p < 0.05 according to region of origin.
Duncans test results are showed with different letters: a.b.c.
Av: Average concentration, min: minimum concentration; Max: maximum concentration and sSD standard deviation.
The identication of all these compounds based on the coincidence of gas chromatographic retention time in DB-WAX column and mass spectrum with those of the pure compounds.

o-Cresol
g-Nonalactone
4-Ethylguaiacol
m-Cresol
4-Propylguaiacol
Ethyl cinnamate
g-Decalactone
4-Ethylphenol
d-Decalactone
4-Vinylguaiacol
2.6-Dimethoxyphenol
Farnesol
4-Vinylphenol
Vanilline
Methyl vanillate
Ethyl vanillate
Acetovanillone
Syringaldehyde

Compound

Table 6. (Continued)

J. Cacho et al.

Flavour Fragr. J. 2012, 27, 322333

Aromatic prole of Peruvian Quebranta piscos

Figure 3. Score plot of principal component analysis applied to quantitative data of Pisco Quebranta varieties from four regions. A = Arequipa, I = Ica,
L = Lima and M = Moquegua. 1 = ethyl butyrate, 2 = butyl acetate, 3 = benzaldehyde, 4 = ethyl furoate, 5 = neryl acetate, 6 = b-phenylethyl acetate,
7 = guaiacol, 8 = m-cresol, 9 = 4-vinylguaiacol, 10 = ethyl vanillate, 11 = methyl acetate, 12 = furfural, 13 = diethyl succinate

Figure 4. Map of Peru showing the locations of the regions considered

in this study

different brandies.[19] This high level of b-phenylethyl acetate

together with the high concentration of b-phenylethanol (previously
mentioned) can be explained by musts rich in phenylalanine
(above all in the case of Quebranta piscos from Lima). Furthermore,
it is well known that variations in the weather may inuence the
amino acid prole.
Geographical Variations

Flavour Fragr. J. 2012, 27, 322333

Copyright 2012 John Wiley & Sons, Ltd.

wileyonlinelibrary.com/journal/ffj

331

Geographical variations are not very strong, since the levels of

just 13 compounds out of the 64 were found to be linked to
the geographical origin. However, it should be remarked that

one of the differences corresponds to the powerful aroma

compound b-phenylethyl acetate, whose levels in piscos from
Arequipa and particularly Moquegua are much smaller than
those found in piscos from Ica and especially Lima. This difference may have sensory relevance. Another difference that may
have some sensory signicance is that of guaiacol, which
presents maxima levels in samples from Ica and minima in
Moquegua and particularly Arequipa. The rest of the geographical differences apply to compounds with poor, if any, sensory
relevance. In spite of that, a principal component study carried
out with the quantitative data of the 13 compounds in the 21
samples, shows that chemical differences may be enough to classify samples attending to their origin. As can be seen in Figure 3,
the two rst components, retaining a 52% of the variance provide
a clear separation of samples from Lima, Ica and from Moquegua
and Arequipa, although differences between these two last origins
are less clear. Neither the third nor the fourth components managed to separate these two regions. This smaller level of difference
may be due to the vicinal proximity between those two regions
which lie in the southern part of Peru (see Figure 4).
The effect of the geographical origin on the sensory properties
of pisco was studied by means of a simple sensory analysis (see
Figure 5). Four regional averaged samples were prepared by
mixing aliquots of all the samples from each region, and the
composite samples were evaluated by a trained panel in nine
aroma attributes. Differences were only found between the
Moquegua sample and all the others. The Moquegua prototype
was characterized by a much higher cut-grass descriptor (55 vs.
less than 20) and by signicant smaller levels of oral, fresh fruit,
raisin and sweet notes, which were in all cases scored under 10,
while in the other samples scores were always higher than 15. It
should be noted that those sensory differences cannot be attributed to differences in a single compound. Even if cis-3-hexenol
has a cut-grass descriptor and is found at maxima levels in the
Moquegua sample, its concentration (152 mg/l) is too low to
cause such an impact. The same happens to hexanol, which is
also found at maxima levels in the Moquegua prototype, but at
levels quite usual and not much higher than those found in
the other regional prototypes. The specic sensory character of

J. Cacho et al.

a)

b)

Arequipa

Oxidized

Nuts

Raisin
30
25
20
15
10
5
0

Raisin
40

Fresh fruit

Floral

Cut grass*

Sweet

d)

Wood

Moquegua
Raisin
60

Fresh fruit

50

Oxidized

Fresh fruit

40
30
20
Floral

Nuts

Floral

10
0

Spicy

Cut grass*

Sweet

Floral

Spicy

Ica

Nuts

10

Nuts

Wood

Raisin
40
35
30
25
20
15
10
5
0

Oxidized

Fresh fruit

30

Cut grass*

c)

Oxidized

20

Spicy

Sweet

Lima

Wood

Spicy

Cut grass*

Sweet

Wood

Figure 5. Graph of mean sensory ratings MF (%) of the piscos from (a) Arequipa, (b) Lima, (c) Ica and (d) Moquegua. *Indicates signicance at p < 0.05

the Moquegua sample can be most likely attributed to the

general lowest level of sweet odorants (b-phenylethyl acetate,
b-phenylethanol, b-damascenone and linalool) and to the highest
level of ethyl acetate found in this sample.

References

Conclusions
The GC-O study has revealed that the Peruvian pisco from
the Quebranta grape variety has a relatively simple aroma
prole formed by 22 odorants, all of which could be identied. Most of the odorants are fermentation related, while guaiacol,
b-damascenone, geraniol and linalool come from the grape. The
chemical analysis of the volatiles of these samples has shown a
volatile prole quite typical of a wine distillate, with not very high
but perceptible levels of linalool, a-terpineol and b-damascenone,
among others. Above all, Quebranta pisco samples are highlighted because of their very high levels of b-phenylethanol and
b-phenylethyl acetate (up to 72 mg/l and 13 mg/l, respectively),
which give rise to key aroma compounds potentially responsible
for deep sensory differences between samples. In fact, the lowest
levels of these compounds and others such as b-damascenone
and linalool can explain the differential sensory character of
Quebranta piscos from the Moquegua region. In general, differences linked to the geographical are not very big, although results
suggest that could be enough for classication.
Acknowledgements

332

The authors are most grateful to the producers who supplied the
different Pisco samples and the Consejo Regulador del Pisc in

wileyonlinelibrary.com/journal/ffj

Peru. Liliana Moncayo thanks the Aragn Institute of Engineering

Research (I3A) for the grant she has received. We also thank the
sniffers from the Laboratory for Flavour Analysis and Enology,
who participated in the GC-O analysis.

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