Eur Food Res Technol (2013) 237:775786

DOI 10.1007/s00217-013-2050-6

ORIGINAL PAPER

Study of the suitability of two hop cultivars for making

herb liqueurs: volatile composition, sensory analysis,
and consumer study
Laura Vazquez-Araujo Raquel Rodrguez-Solana
Sandra M. Cortes-Dieguez Jose M. Domnguez

Received: 5 April 2013 / Revised: 15 May 2013 / Accepted: 15 June 2013 / Published online: 4 July 2013
 Springer-Verlag Berlin Heidelberg 2013

Abstract The suitability of two different cultivars of hop

for making herb liqueurs was evaluated in the present study.
Grape distillate marc was used to macerate the hop
(15 g L-1), and headspace-solid phase microextraction was
conducted to determine which volatile compounds migrated
from the hop flowers to the liqueur. Also, a descriptive
sensory analysis and a consumer study were conducted,
with 7 herb liqueurs which had different percentages of hop
liqueurs, to determine the acceptability of the product and
the liking drivers. Saaz cultivar proved to be a good option
to improve or develop herb liqueurs, because the samples
which had a 10 and 25 % of Saaz liqueur were the most
liked for consumers. Samples which had Nugget liqueur
resulted too bitter and with an excess of herb flavor for
consumers, maybe because of the high concentration of
phenolic compounds or the presence of high amounts of
certain aromatic compounds (e.g., myrcene, humulene).
Saaz hop increased the intensity of aromatic herbs flavor
and decreased the perception of excess of sweetness of the
commercial liqueur. The addition of this cultivar could
contribute with new aromatic notes to a product, bringing to
the liqueur unique characteristics.

L. Vazquez-Araujo (&)
R. Rodrguez-Solana

S. M. Cortes-Dieguez
J. M. Domnguez
Chemical Engineering Department, Faculty of Sciences,
University of Vigo, Campus Ourense, As Lagoas s/n,
32004 Ourense, Spain
e-mail: lvazquezara@uvigo.es
L. Vazquez-Araujo
R. Rodrguez-Solana

S. M. Cortes-Dieguez
J. M. Domnguez
Laboratory of Agro-food Biotechnology, CITI-University
of Vigo, Tecnopole-Tecnological Park of Galicia,
San Cibrao das Vinas, Ourense, Spain

Keywords Humulus lupulus L.
Nugget
Saaz
Sensory

analysis
Phenolic compounds
HS-SPME

Introduction
Herb spirits have been made and consumed for centuries in
different European countries. These liqueurs are generally
made by macerating different aromatic herbs in fermented
grape marc distillate, distilling the fermented grape marc in
the presence of herbs, adding herbal extracts to the distilled
alcohol, or combining some of these methodologies. Different types and brands can be found across Europe, for
example, Italians Galliano and Strega, German Krauterlikor, French Chartreuse, and Spanish Orujo de Hierbas.
In Galicia (Spain), in 2004, the herb liqueurs were
included in the list of the products covered by the Geographical Designation of the Spirits and Traditional
Liqueurs from Galicia [1]. The regulation which defines
the characteristics of the Traditional Liqueurs from Galicia
includes some physico-chemical and sensory requirements,
highlighting that (1) the liqueur has to be made with at least
3 different aromatic herbs, (2) the liqueur must have
between 20 and 40 % alcohol by volume (abv), and (3) the
liqueur needs to meet certain sensory characteristics:
translucent and clean appearance, color between straw
yellow to greenish yellow; intense, fine, delicate, tasty, and
ample aroma, with floral and balsamic notes, and also
reminding the original grape marc spirit which completes
the herb notes which are characteristic of the product; it
should have absence of musty, burnt, acetic, and dirty
notes [2]. Therefore, to commercialize the herb liqueurs
with the Traditional Liqueur from Galicia label, the
product has to be evaluated by the official tasting panel of
the regulating council.

123

776

Prior to 2012, only some herbs/spices have been

authorized to make the liqueurs: mint, chamomile, lemon
verbena, rosemary, oregano, thyme, coriander, orange
blossom, fennel, licorice, nutmeg, and cinnamon. However,
from 2012, new regulations authorized the use of any kind
of herb which is suitable for human consumption [2].
The aims of the present study are to investigate whether
hop is suitable for making herb liqueurs and to determine
whether the aromatic notes which this ingredient can bring
to the final product are liked or disliked by consumers. Hop
cones, the immature inflorescences of the female plant of
Humulus lupulus L., are widely used to enhance the flavor
and bitterness of beer. With only a small amount of this
ingredient, different aromatic notes could be added to the
liqueur: green and grassy notes which come from different
aldehydes (e.g., hexanal); citrus, floral, and fruity aromas
originated from esters and compounds such as nerol or
linalool; or even typical herbal notes from oxidized sesquiterpenes [3].
There are a small number of studies which determine the
volatile composition of aromatic herbs, including hop [46]
and grape marc spirits [7], but no research can be found in
the current literature which details the volatile composition
of herb liqueurs. Some authors have reported different key
odorants of beer which come from hop: linalool (floral),
myrcene (geranium), geraniol (floral), ethyl 2-methylbutanoate (citrus, apple-like), ethyl 3-methylbutanoate (citrus,
sweet), and ethyl 2-methylpropanoate (citrus, pineapple)
[8, 9].
It would be interesting to determine whether these volatile compounds can be found in the herb liqueur made
with hop, and also to study whether they have the same
importance. Headspace-solid phase microextraction
(HS-SPME) has been successfully employed in previous
researches to determine the volatile composition of hop
[6, 10] and also raw spirits [11, 12]; therefore, this technique was chosen for the present study.

Materials and methods

Hop Samples
Hop samples were kindly provided by the company Hijos
de Rivera Inversiones Corporativas S.L (Gambrinus 2-10,
Pol. Ind. Grela. A Coruna, Spain). The samples were the
immature inflorescences of the female plant of Humulus
lupulus L., recently harvested and dried. Two hop cultivars,
which were grown in the same area (A Coruna, Galicia,
NW Spain), were chosen for the study: Nugget and Saaz.
Korfta et al. [13] studied different quality parameters
of some hop varieties, and reported a classification of
cultivars into four groups: fine aroma, aroma, bittering

123

Eur Food Res Technol (2013) 237:775786

dual-purpose (aroma and bitterness), and high-alpha hops

(bittering). Saaz can be classified as a fine aroma or
aroma cultivar, and Nugget is an example of high
alpha hop cultivar, although Nugget was reported as
having high concentration of volatile compounds as well
[6].
Herb liqueurs preparation
Twenty-five liters of grape marc distillate (65.5 % abv)
was provided by the company Hijos de Rivera Inversiones
Corporativas S.L., which also gave a similar amount of
commercial herb liqueur (made with the same grape marc
distillate). For the maceration of hop, 15 g of each cultivar, and also a combination of both cultivars (7.5 g
Saaz ? 7.5 g Nugget), was added per liter of grape marc
distillate (obtaining Nugget liqueur, Saaz liqueur,
and N ? S liqueur). A total of 5 L of each hop liqueur
was macerated during 3 weeks at approximately 21 C,
using 3 different jars for liqueur (3 replications), and
avoiding leaving too much headspace in the jars. After
these 3 weeks of maceration, the liqueurs were filtered
(Whatman n81 filter, cellulose, 11 lm) and kept at 4 C
during 24 h for stabilization. After this time, the liqueurs
were adjusted to 30 % abv and approximately 200 g
sucrose L-1 by adding sucrose and distillate water,
obtaining products with the same characteristics of the
commercial liqueur.
Once the hop liqueurs were made, total phenolic content
(TPC) and headspace-solid phase microextraction were
conducted to characterize all samples (commercial and hop
liqueurs). Then, mixtures of the hop liqueurs with the
commercial sample were prepared to conduct the sensory
analyses.
Total phenolic content
Total phenolic content was measured as indicator of the
antioxidant activity in the liqueurs. TPC was determined by
using the FolinCiocalteu method reported by VazquezAraujo et al. [14], which was based on the one reported by
Skinkard and Singleton [15], with some modifications.
Results were expressed as mg of gallic acid equivalents per
L of liqueur. Experiments were run in triplicate.
Volatile composition of the hop samples
and the liqueurs
Solid phase microextraction
Headspace of the hop cultivar samples, and also of the
different liqueurs, was studied using the semi-quantitative
technique solid phase microextraction (SPME).

776

Prior to 2012, only some herbs/spices have been

authorized to make the liqueurs: mint, chamomile, lemon
verbena, rosemary, oregano, thyme, coriander, orange
blossom, fennel, licorice, nutmeg, and cinnamon. However,
from 2012, new regulations authorized the use of any kind
of herb which is suitable for human consumption [2].
The aims of the present study are to investigate whether
hop is suitable for making herb liqueurs and to determine
whether the aromatic notes which this ingredient can bring
to the final product are liked or disliked by consumers. Hop
cones, the immature inflorescences of the female plant of
Humulus lupulus L., are widely used to enhance the flavor
and bitterness of beer. With only a small amount of this
ingredient, different aromatic notes could be added to the
liqueur: green and grassy notes which come from different
aldehydes (e.g., hexanal); citrus, floral, and fruity aromas
originated from esters and compounds such as nerol or
linalool; or even typical herbal notes from oxidized sesquiterpenes [3].
There are a small number of studies which determine the
volatile composition of aromatic herbs, including hop [46]
and grape marc spirits [7], but no research can be found in
the current literature which details the volatile composition
of herb liqueurs. Some authors have reported different key
odorants of beer which come from hop: linalool (floral),
myrcene (geranium), geraniol (floral), ethyl 2-methylbutanoate (citrus, apple-like), ethyl 3-methylbutanoate (citrus,
sweet), and ethyl 2-methylpropanoate (citrus, pineapple)
[8, 9].
It would be interesting to determine whether these volatile compounds can be found in the herb liqueur made
with hop, and also to study whether they have the same
importance. Headspace-solid phase microextraction
(HS-SPME) has been successfully employed in previous
researches to determine the volatile composition of hop
[6, 10] and also raw spirits [11, 12]; therefore, this technique was chosen for the present study.

Materials and methods

Hop Samples
Hop samples were kindly provided by the company Hijos
de Rivera Inversiones Corporativas S.L (Gambrinus 2-10,
Pol. Ind. Grela. A Coruna, Spain). The samples were the
immature inflorescences of the female plant of Humulus
lupulus L., recently harvested and dried. Two hop cultivars,
which were grown in the same area (A Coruna, Galicia,
NW Spain), were chosen for the study: Nugget and Saaz.
Korfta et al. [13] studied different quality parameters
of some hop varieties, and reported a classification of
cultivars into four groups: fine aroma, aroma, bittering

123

Eur Food Res Technol (2013) 237:775786

dual-purpose (aroma and bitterness), and high-alpha hops

(bittering). Saaz can be classified as a fine aroma or
aroma cultivar, and Nugget is an example of high
alpha hop cultivar, although Nugget was reported as
having high concentration of volatile compounds as well
[6].
Herb liqueurs preparation
Twenty-five liters of grape marc distillate (65.5 % abv)
was provided by the company Hijos de Rivera Inversiones
Corporativas S.L., which also gave a similar amount of
commercial herb liqueur (made with the same grape marc
distillate). For the maceration of hop, 15 g of each cultivar, and also a combination of both cultivars (7.5 g
Saaz ? 7.5 g Nugget), was added per liter of grape marc
distillate (obtaining Nugget liqueur, Saaz liqueur,
and N ? S liqueur). A total of 5 L of each hop liqueur
was macerated during 3 weeks at approximately 21 C,
using 3 different jars for liqueur (3 replications), and
avoiding leaving too much headspace in the jars. After
these 3 weeks of maceration, the liqueurs were filtered
(Whatman n81 filter, cellulose, 11 lm) and kept at 4 C
during 24 h for stabilization. After this time, the liqueurs
were adjusted to 30 % abv and approximately 200 g
sucrose L-1 by adding sucrose and distillate water,
obtaining products with the same characteristics of the
commercial liqueur.
Once the hop liqueurs were made, total phenolic content
(TPC) and headspace-solid phase microextraction were
conducted to characterize all samples (commercial and hop
liqueurs). Then, mixtures of the hop liqueurs with the
commercial sample were prepared to conduct the sensory
analyses.
Total phenolic content
Total phenolic content was measured as indicator of the
antioxidant activity in the liqueurs. TPC was determined by
using the FolinCiocalteu method reported by VazquezAraujo et al. [14], which was based on the one reported by
Skinkard and Singleton [15], with some modifications.
Results were expressed as mg of gallic acid equivalents per
L of liqueur. Experiments were run in triplicate.
Volatile composition of the hop samples
and the liqueurs
Solid phase microextraction
Headspace of the hop cultivar samples, and also of the
different liqueurs, was studied using the semi-quantitative
technique solid phase microextraction (SPME).

Eur Food Res Technol (2013) 237:775786

The flowers were milled before its study, for 20 s in a

coffee grinder (Moulinex, Groupe SEB, Mexico) guaranteeing similar particle size for both samples. A quarter
gram of each sample was placed in a 10 mL vial with a
polypropylene hole cap PTFE/silicone septa. Vials were
equilibrated for 10 min at 40 C in a water bath. After this
equilibration time, a 50/30 lm DVB/CAR/PDMS fiber was
exposed to the sample headspace for 15 min at 40 C.
Goncalves et al. [16] reported that the fiber DVB/CAR/
PDMS presented the best extraction efficiency when
studying terpenoid metabolites in hop essential oil, and also
that the addition of salt or agitation of the sample led to a
decrease in the chromatographic peak areas, for that reason, no salt was added and the sample was not stirred. After
sampling, the desorption of analytes from the fiber coating
was made in the injection port of the GC at 250 C, during
2 min, in splitless mode. Experiments were run in triplicate
for each cultivar sample.
The herb liqueurs volatile composition was studied
adapting the methodology reported by Plutowska and
Wardencki [11, 12]. Exactly 3.7 mL of liqueur with
1.30 mL of distillate water and 0.5 g NaCl was placed in a
10 mL vial with a polypropylene hole cap PTFE/silicone
septa. Vials were equilibrated for 10 min at 45 C in a
water bath and agitated using a magnetic stirrer (600 rpm).
After this equilibration time, a 50/30 lm DVB/CAR/
PDMS fiber was exposed to the sample headspace for
40 min, at 45 C, and constantly stirred at 600 rpm. After
sampling, the desorption of analytes from the fiber coating
was made in the injection port of the GC at 250 C, during
2 min, in splitless mode. Experiments were run in triplicate
for each liqueur (commercial, Nugget, Saaz, and N ? S).
Chromatographic analyses
A gas chromatograph (Agilent GC 7820A; Agilent technologies, Santa Clara, CA, USA), coupled with an Agilent
mass spectrometer detector (5975 Series MSD), was used
to isolate and identify the volatile compounds. The GCMS
system was equipped with a HP-5MS column (30 m 9
0.25 mm 9 0.25 lm film thickness). The temperature of
the column began at 50 C and held for 1 min, increased
1 C per minute to 90 C and then 2 C per minute to
140 C. Then, temperature was increased 40 C per minute
to 250 C and held at this temperature during 1.25 min.
The constant column flow was 1.2 ml min-1, using
hydrogen as the carrier gas, and the injection port was at
250 C.
Most compounds were identified using two different
analytical methods: (1) Kovats indexes and (2) mass
spectra (authentic chemicals and Wiley spectral library
collection). Also, standards of limonene, b-myrcene,
a-humulene, ocimene, b-caryophyllene, caryophyllene

777

oxide, and methyl nonanoate (Sigma-Aldrich Co., St.

Louis, MO) were used to ensure the identification of some
compounds. Identification was considered tentative when
based entirely on mass spectral data.
Sensory analyses
Sensory evaluation with trained panel
Seven highly trained panelists from the Regulating Council
of the Geographical Designation of the Spirits and Traditional Liqueurs from Galicia participated in this study,
testing the same samples which were evaluated for consumers. Because the traditional herb liqueurs are made with
a combination of at least 3 different herbs, the consumer
study was conducted with the following 7 samples (coded
as indicated):

Sample A: commercial sample (which already have a

combination of at least 3 aromatic herbs)
Sample B: mixture of 90 % commercial ? 10 % Saaz
liqueur samples
Sample C: mixture of 75 % commercial ? 25 % Saaz
liqueur samples
Sample D: mixture of 90 % commercial ? 10 %
Nugget liqueur samples
Sample E: mixture of 75 % commercial ? 25 % Nugget liqueur samples
Sample F: mixture of 90 % commercial ? 10 %
(N ? S) liqueur samples
Sample G: mixture of 75 % commercial ? 25 %
(N ? S) liqueur samples

Each panelist had more than 80 h of training in sensory

testing and more than 300 h of testing experience with
grape marc distillates, and herbs and coffee liqueurs. All
samples were poured into the official tasting glass for
evaluation. Each panelist received *15 mL of each
product for evaluation. The samples were served at 4 C.
Table 1 shows the terms and definitions used for the
evaluation, terms which corresponded to the lexicon
developed by the panel to evaluate herb liqueurs for the
Regulating Council. A numerical scale from 0 (representing none) to 9 (representing extremely strong) was
used in this study. The testing room was at 21 1 C and
55 5 % of RH, and the illumination was a combination
of natural and nonnatural (fluorescent) light.
Consumer study
A group of 153 consumers, aged 1875, were recruited in
two different areas of Spain (NW and SE) to conduct the
study (77 and 76 consumers, respectively). The northwestern area of Spain is well recognized by having an

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Eur Food Res Technol (2013) 237:775786

Table 1 Attributes and definitions used by the trained panel

Definition
Flavor
Sweet

The fundamental taste factor associated with a sucrose solution

Sour

The fundamental taste factor associated with a citric acid solution

Salty

The fundamental taste factor of which sodium chloride is typical

Bitter

The fundamental taste factor associated with a caffeine solution

Aromatic herbs

The aromatics associated with commonly known aromatic herbs such as fennel, mint, and coriander

Mint

The aromatics associated with mint

Chamomile

The aromatics associated with chamomile

Lemon verbena

The aromatics associated with lemon verbena

Rosemary

The aromatics associated with rosemary

Oregano
Fennel

The aromatics associated with oregano

The aromatics associated with fennel

Coriander

The aromatics associated with coriander

Thyme

The aromatics associated with thyme

Floral

Sweet and perfume-like impression associated with flowers such as orange blossom, roses, or hyacinth

Fruity (not citrus)

The aromatics associated with pome and stone fruits, such as apple and pear

Fruity (citrus)

The aromatics associated with commonly known citrus fruits, such as lemons, limes, or oranges

Spicy

The aromatics associated with spices such as cinnamon, nutmeg or licorice

Balsamic

The aromatics associated with eucalypt, causing a refreshing sensation in the mouth

Honey-like

The aromatics typical of honeys and molasses

Grape marc

The aromatics typical of the distillate grape marc used to macerate the herbs

Herbaceous

The aromatics caused by the presence of hexanals generated during the marcs storage

Alcoholic

Ethanol aroma

Cellulose

The aromatics which reminds paper or cardboards

Sulfur compounds

The aromatics associated with cooked or spoiled eggs

Mouthfeels
Astringent

The dry puckering mouthfeel due to the presence of certain substances such as tannins
or polyphenols in the mouth

Pungent

Bitting tactile sensation due to the presence of certain compounds such as ethanol and black pepper

Drying

Dry sensation in the mouth due to the presence of ethanol

Alcoholic sensation

Ethanolic sensation in the mouth. It could be warm if the sensation is low, to burning
if it is a high sensation

Greasiness

Coating sensation in the mouth

Global assessment
Balanced

If the product does not have any aromatic note with highlights over the set, it receives a high score
in balance; otherwise, it would receive a low score in the scale

Structured

Term used to discern the weight of the liquid and how it feels in the mouth. Light means a low
score in structure; full body means a high score in structure

important tradition in making and consuming grape marc

distillate and its derivatives: herbs and coffee liqueurs. The
southwestern area of Spain was chosen to give a comparison with an area which does not have such a traditional
links with herb liqueurs. The gender ratio was approximately 45 % females and 55 % males. Ages were distributed, and all of them were represented in both areas of the
country.

123

Consumers were recruited from the local areas and were

asked to attend to just one session. Both consumer studies
were carried out in the testing rooms of two universities:
University of Vigo (Ourense, NW Spain) and Miguel
Hernandez University (Escuela Politecnica Superior de
Orihuela, Orihuela, SE Spain); they needed to be willing to
try herb liqueurs and consume distillates or liqueurs at least
34 times/month. Each consumer tested all seven samples

Eur Food Res Technol (2013) 237:775786

in a single session, carried out in a temperature controlled

room (21 1 C) with a combination of natural and
nonnatural (fluorescent) light. The presentation order was
randomized using a modified Williams Latin square
design s. Approximately 8 mL of each sample were served
at 4 C in 100 ml disposable plastic cups, waiting all time
requested by the consumer between samples. Consumers
were instructed to give a sip and answer the questions.
More sample was available for them if requested. Also,
consumers were asked to eat unsalted crackers and drink
deionized water at room temperature for palate cleansing
in-between samples.
The consumers were asked to evaluate the overall liking
of the samples on a 9-point hedonic scale (1 = dislike
extremely to 9 = like extremely) and similar hedonic
scales for some attributes: sweetness, bitterness, and aromatic herb flavor. Just-about-right (JAR) questions about
the aforementioned attributes were done as well, using a
9-point scale where 5 corresponded to the JAR score. A
parallel questionnaire about demographic information was
also asked to determine possible relationships or differences among demographic groups.
Data analyses
All data were subjected to statistical analysis using SPSS
(version 19.0; SPSS Inc., Chicago, Ill.), used for analysis of
variance (ANOVA) and Tukeys honestly significant differences (HSD) for post hoc mean separation. Also, internal preference maps and partial least square regression
(PLS regression map, with the intent of relating consumer
results with descriptive data) were conducted using the
Unscrambler version 9.7 (Camo Software, Oslo, Norway).

Results and discussion

Differences between hop cultivars
Table 2 shows the main differences in the volatile composition of the headspace of Nugget and Saaz hop cultivars.
Both cultivars were characterized by having high proportions of terpenes (more than 50 % of the total area of
volatiles was composed by terpenes) and sesquiterpenes
(more than 35 %). Main differences were found in the
esters fraction of both samples, highlighting that Nugget
cultivar had a higher amount of esters: 12.2 % of the total
area of volatiles in Nugget and only 6.38 % in Saaz.
Vazquez-Araujo et al. [6] reported similar results when
studying hop pellet samples, in which Nugget cultivar had
approximately double the content of ester compounds than
Saaz. Proportions of other groups of compounds are not in
agreement with the ones reported previously by these

779

authors, maybe because the present study was conducted

with hop flowers and Vazquez-Araujo et al. [6] studied hop
pellets. As reported by Krofta [13], and then confirmed by
Vazquez-Araujo et al. [6], results of the present study
showed that there were substantial differences between the
terpenic fraction of these hop cultivars: Saaz (fine aroma
variety) had significant amounts of (Z,Z)-a-farnesene, (E)b-farnesene (apple, lavender, etc.), b-bisabolene (floral,
freesia, etc.), and (E,E)-a-farnesene [17], volatile compounds not present in the Nugget sample (bitter variety).
Differences among liqueurs
Regarding the liqueurs, Table 3 shows the differences
among the TPC in the liqueurs used to elaborate the final
herb liqueurs with hop. As shown in the table, all samples
were significantly different (p \ 0.05), being the commercial liqueur the one which had the lowest TPC (ca
205 mg gallic acid equivalents L-1). Nugget cultivar
brought the highest amount of phenolic compounds to the
grape distilled marc (ca 332 mg gallic acid equivalents
L-1). Therefore, it is expected that using hop as an ingredient to make herb liqueurs will slightly increase the TPC
and also the antioxidant activity of the end product. Roby
et al. [18] reported that methanol and ethanol were the best
extracting solvents for phenolics in plants such as thyme,
sage, and marjoram. Because of the high amount of ethanol
in the grape distillate marc used to macerate the herbs,
most phenolic compounds migrated from the plant to the
liqueur, providing a high antioxidant activity to the
product.
When looking at the aromatic profile of the liqueurs
made with Nugget or Saaz hop cultivars, significant differences were found if when compared with the aromatic
profiles of the flowers (Tables 4, 2). After the maceration
process, Saaz liqueur was characterized by its high proportion of esters (62 %), but Nugget liqueur was characterized by having a high proportion of terpenes (ca 32 %)
and sesquiterpenes (ca 49 %). Vazquez-Araujo et al. [6]
reported that the volatile profile of hop obtained using HSSPME or hydrodistillation was different if looking at the
behavior of some chemical groups. Because esters were
pretty instable compounds, a great variation was observed
within the chemical group, and no pattern was observed
when comparing both extraction techniques. Something
similar might be happening in the present study, because
the maceration could be considered a solidliquid extraction technique. Also, not all hop cultivars have same
amount of essential oil (varying from 0.5 to 2 %), so the
amount of volatile compounds extracted by the ethanol
during the maceration of the hop flowers might vary. If
looking at the total areas accounts of the chromatograms
obtained using GCMS, Saaz cultivar had a significant

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Table 2 Volatile compounds of the hop flowers (area %)

Compound

KIa (NIST)

KI (Exp)

Nugget

Saaz

Esters
1

2-Methyl-, 3-methylbutyl propanoate

1017

1016

1.57 0.19

n.d.

2-Methyl-, 2-methylbutyl propanoate

1014

1019

1.86 0.20

n.d.

Methyl heptanoate

1026

1025

1.49 0.15

1.58 0.41

2-Methyl-, 2-methylbutyl butanoate

1110

1103

0.20 0.03

n.d.

3-Methyl-, 2-methylbutyl butanoate

1110

1107

0.40 0.04

n.d.

Methyl octanoate

1125

1124

2.68 0.14

1.97 0.06

2-Methyl-, hexyl propanoate

1149

1146

0.11 0.01

n.d.

Methyl benzeneacetate

1180

1171

0.03 0.01

0.02 0.01

1195

1205

0.04 0.01

n.d.

1225

1210
1224

0.14 0.01
0.76 0.03

0.08 0.01
0.64 0.02

1227

0.03 0.01

n.d.

1246

0.05 0.01

n.d.

Ethyl octanoate

10
11

Methyl n-nonenoate
Methyl nonanoate

12

Methyl n-nonenoate

13

2-Methyl-, heptyl propanoate

1248

14

Isopentyl hexanoate

1254

15

Methyl n-decanoate

1251

n.d.

0.01 0.01

1309

1.85 0.11

1.57 0.07

16

Methyl geranate

1331

1322

0.16 0.03

0.11 0.01

17

Methyl decanoate

1326

1327

0.85 0.03

0.40 0.04

12.2

6.38

Terpenes
1

Myrcene

p-Cymene

991

998

44.3 2.0

55.0 0.3

1028

1021

0.16 0.04

n.d.

Limonene

1034

1024

2.07 0.06

0.80 0.08

(E)-b-Ocimene

1044

1034

0.38 0.01

0.18 0.04

(Z)-b-Ocimene

1049

1044

3.51 0.07

0.74 0.19

c-Terpinene

1064

1050

0.10 0.01

0.13 0.01

Allo-ocimene

1130

1134

0.37 0.02
50.9

0.14 0.05
57.0

Linalool

1107

1099

1.32 0.11

0.50 0.01

Terpenoids
1

Sesquiterpenes
1

a-Cubebene

1345

1338

0.16 0.03

0.10 0.01

Sativene

1394

1349

0.05 0.01

0.02 0.01

a-Ylangene

1370

1357

0.20 0.01

0.14 0.01

a-Copaene

1377

1362

0.58 0.03

0.45 0.01

(Z)-b-Caryophyllene

1405

1390

0.56 0.12

0.10 0.03

(E)-b-Caryophyllene

1418

1403

12.8 0.5

6.97 0.15

b-Copaene

1422

1411

1.04 0.15

0.42 0.08

(Z,Z)-a-Farnesene

1462

1430

n.d.

1.03 0.10

Humulene

1457

1441

16.9 0.6

16.2 0.2

10

Caparratriene

1493

1446

n.d.

0.42 0.19

11
12

(E)-b-Famesene
b-Selinene

1461
1490

1460
1469

n.d.
0.87 0.02

8.63 0.94
0.17 0.01

13

a-Selinene

1498

1478

0.86 0.02

0.14 0.01

14

()-Cadinene

1523

1486

0.12 0.01

0.08 0.01

15

a-Muurolene

1483

1488

0.13 0.01

0.11 0.01

16

c-Cadinene

1504

1498

0.36 0.01

0.36 0.01

17

b-Bisabolene

1516

1500

n.d.

0.07 0.01

123

Eur Food Res Technol (2013) 237:775786

781

Table 2 continued
Compound

KIa (NIST)

KI (Exp)

Nugget

Saaz

18

(E,E)-a-Farnesene

1508

1504

n.d.

0.14 0.01

19

(E)-Calamenene

1505

1506

0.08 0.01

n.d.

20

(Z)-Calamenene

1520

1508

0.10 0.02

0.10 0.01

21

d-Cadinene

1525

1511

0.61 0.03

0.55 0.01

22

a-Calacorene

1542

1527

0.03 0.01

n.d.

35.5

36.1

0.01 0.01

0.03 0.01

Sesquiterpenoids
1

Caryophyllene oxide

1582

1590

n.d., not detected; n.a., not available for HP5-MS or equivalent column. Retention indexes reported for the HP-5MS or equivalent column. Data
mean of 3 replications
a

NIST [24]

lower area counts than Nugget, which seemed to show that

Nugget cultivar brought a higher amount of volatile compounds to the liqueur.
Nance and Setzer [19] reported that, in general, hop oils
rich in monoterpenoids are fruity or citrusy, while those
dominated by sesquiterpenes tend toward earthy, herbal,
woody, or spicy aromas. Nugget and Saaz liqueurs were
similar if looking at the proportion terpenes: sesquiterpenes, but qualitative differences were found related to the
compounds which were present in one or another sample,
e.g., presence of c-terpinene and allo-ocimene in Nugget
and not in Saaz liqueur, or presence of (E)-b-farnesene and
b-bisabolene in Saaz and not in Nugget liqueur. All those
differences could be translated into sensory differences of
the liqueurs.
Commercial liqueur was characterized by having a high
proportion of esters (e.g., ethyl octanoate and ethyl decanoate), mainly coming from the grape distillate marc
used as raw material [7]. Also, highlighted the presence of
phenyl derivatives such as E-anethole and p-propylanisole,
compounds typically found in fennel [20, 21]. The presence of certain terpenoids such as isomenthol, levomenthol, or eucalyptol suggested the presence of mint as other
ingredient of the commercial liqueur [22].

notes, and also in the astringency and pungency mouthfeels. Results seemed to indicate that Nugget hop brought
some negative notes to the product: higher bitterness,
astringency, pungency, herbaceous aromas, and alcoholic
sensation. According to the literature, at least in some
juices, a high content on phenolic compounds is related to
sensory parameters such as astringency and bitterness [23].
Therefore, it was expected that liqueur with a high concentration of Nugget hop liqueur had higher intensities of
these attributes (Table 3). Also, although no significant
differences were found (p C 0.05) among samples,
liqueurs with a higher amount of Nugget hop liqueur
received higher scores in the fruity-citrus notes, maybe due
to its high content of terpenes [19]. Commercial liqueur
was characterized by having chamomile, lemon verbena,
and aromatic herbs notes, as well as a higher sweetness
than all other samples (although the sugar content was the
same in all samples).
Results of the consumer study showed no significant
differences (p C 0.05) between consumers from both areas
of the country or between genders, so data were treated as a
unique group. Two groups of samples were observed when
analyzing the results of the overall liking of the products:
samples A, B, C, and F (with scores close to 6 in a 9 points

Sensory analyses results

Table 3 Total phenolic content of the liqueurs

Figure 1 shows the flavor profiles of 3 of the 7 samples: A

(commercial), C (?25 % Saaz liqueur), and D (?25 %
Nugget liqueur). These samples exhibited the most sensory
significant differences and as such are the only ones represented in the spider plot. All other samples received
sensory scores between one of the samples showed in the
graph (the % of hop liqueur addition to the commercial
sample was lower). Significant differences (p \ 0.05) were
found for these 3 samples in sweet, bitter, mint, chamomile, lemon verbena, balsamic, herbal, and alcoholic flavor

Liqueur

Total phenolic content (mg

Gallic acid equivalents L-1)

Commercial

205 9d

Saaz

246 7c

Nugget

332 24a

Nugget ? Saaz

288 6b

Data mean of 3 replications. Values followed by the different letter,

within the same variation source, were significantly different
(p \ 0.05). Tukeys honestly significant differences (HSD)

123

782

Eur Food Res Technol (2013) 237:775786

Table 4 Volatile compounds of the commercial sample and the hop liqueurs (area %)
Compound

KIa (NIST)

KI (Exp.)

Commercial

Nugget

Ethyl hexanoate

996

1002

2.36 0.51

n.d.

3.65 0.20

n.d.

2-Methyl-, 3-methylbutyl propanoate

1017

1013

n.d.

0.36 0.02

n.d.

0.25 0.02

Saaz

Nugget ? Saaz

Esters

2-Methyl-, 3-methylbutyl propanoate

1014

1015

n.d.

0.80 0.06

n.d.

0.53 0.01

Methyl heptanoate

1026

1022

n.d.

0.62 0.03

0.34 0.02

0.52 0.03

Ethyl heptanoate

1097

1099

n.d.

0.08 0.01

0.08 0.01

0.10 0.01

2-Methyl-, 2-methylbutyl butanoate

1110

1103

n.d.

0.07 0.01

n.d.

n.d.
0.14 0.01

3-Methyl-, 2-methylbutyl butanoate

1110

1107

n.d.

0.16 0.01

n.d.

Methyl octanoate

1125

1123

0.14 0.02

0.97 0.03

0.60 0.03

0.86 0.02

2-Methyl-, hexyl propanoate

1149

1146

n.d.

0.05 0.01

n.d.

0.03 0.01

10

Ethyl octanoate

1195

1205

30.1 0.9

10.5 0.2

24.9 1.0

16.5 0.1

11

Methyl n-nonenoate

1212

n.d.

0.07 0.01

0.04 0.01

0.06 0.01

12

Methyl nonanoate

1225

1224

n.d.

0.42 0.04

0.31 0.01

0.42 0.01

13

2-Methyl-, heptyl propanoate

1248

1246

n.d.

0.04 0.01

n.d.

0.03 0.01

14

Isopentyl hexanoate

1254

15

Ethyl n-nonenoate

1248

0.08 0.01

0.04 0.01

0.12 0.01

0.07 0.01

1285

n.d.

n.d.

0.02 0.01

n.d.

16

Menthol, acetate

1294

1288

0.73 0.03

n.d.

n.d.

n.d.

17

Ethyl nonanoate

1294

1298

0.21 0.01

0.15 0.01

0.44 0.01

0.25 0.01

18

Methyl n-decanoate

1310

n.d.

1.33 0.09

0.80 0.08

1.29 0.05

19

Methyl geranate

1331

1323

n.d.

0.14 0.01

0.12 0.02

0.14 0.01

20

Methyl decanoate

1326

1327

0.16 0.01

0.80 0.06

0.81 0.06

0.87 0.03

21

2-Butyl octanoate

n.a.

1351

0.03 0.01

n.d.

0.07 0.01

0.05 0.01

22

Ethyl decanoate

1394

1409

26.7 0.8

1.58 0.03

26.3 1.8

9.52 1.10

23

3-Methylbutyl octanoate

1446

1451

0.27 0.02

0.12 0.01

0.34 0.02

0.20 0.01

24

2-Methylbutyl octanoate

1449

1452

0.08 0.01

n.d.

n.d.

n.d.

25

Isobutyl n-caproate

1545

1548

0.03 0.01

n.d.

n.d.

n.d.

26

Ethyl dodecanoate

1576

1600

4.48 0.42

0.91 0.10

3.12 0.54

1.56 0.12

27

3-Methylbutyl pentadecanoate

1644

1650

0.09 0.01

n.d.

n.d.

n.d.

28

Ethyl tetradecanoate

1793

1797

0.16 0.02

n.d.

n.d.

n.d.

29

Ethyl hexadecanoate

1993

1970

0.06 0.01

n.d.

n.d.

n.d.

65.6

19.2

62.0

33.4

Phenyl derivatives
1

E-3-Caren-2-ol

1111 (DB1)

1019

0.44 0.19

n.d.

n.d.

n.d.

Estragole

1196

1189

0.47 0.02

n.d.

n.d.

n.d.

p-Propylanisole

n.a.

1199

5.41 0.30

n.d.

n.d.

n.d.

(Z)-Anethole

1258

1243

1.04 0.09

n.d.

n.d.

n.d.

(E)-Anethole

1283

1275

21.9 1.9

0.09 0.03

0.07 0.01

0.05 0.01

Dihydrosafrole

n.a.

1285

0.37 0.03

n.d.

n.d.

n.d.

29.7

0.09

0.07

0.05

n.d.

29.9 0.4

13.9 0.7

25.5 0.7

Terpenes
1

b-Myrcene

991

1000

p-Cymene

1028

1017

0.31 0.12

n.d.

n.d.

n.d.

Limonene

1034

1021

n.d.

0.31 0.04

0.16 0.01

0.17 0.01
0.11 0.01

(E)-b-Ocimene

1044

1033

n.d.

0.13 0.01

0.05 0.01

(Z)-b-Ocimene

1049

1042

n.d.

1.33 0.01

0.21 0.01

0.87 0.05

c-Terpinene

1064

1049

1.15 0.42

0.04 0.01

n.d.

0.04 0.01

n.d.

Allo-ocimene

1130

1134

n.d.

0.12 0.01

p-Menthone

1153

1141

0.77 0.03

n.d.

n.d.

n.d.

2.22

31.8

14.3

26.8

123

0.10 0.01

Eur Food Res Technol (2013) 237:775786

783

Table 4 continued
Compound

KIa (NIST)

KI (Exp.)

Commercial

Nugget

Saaz

Nugget ? Saaz

Terpenoids
1

Eucalyptol

1038

1021

0.68 0.13

n.d.

n.d.

n.d.

Terpinolene

1090

1078

0.16 0.04

n.d.

n.d.

n.d.

Linalool

1102

1098

0.32 0.04

n.d.

n.d.

n.d.

Camphor

1138

1130

0.12 0.02

n.d.

n.d.

n.d.

Z-p-Menth-2-en-1-ol

1139

1151

0.18 0.01

n.d.

n.d.

n.d.

Citronellal

1150

1152

0.14 0.01

n.d.

n.d.

n.d.

Levomenthol

1172

1163

0.25 0.09

n.d.

n.d.

n.d.

Isomenthol

1179

1164

0.42 0.08

n.d.

n.d.

n.d.

Isopulegol

1148

1166

0.16 0.05

n.d.

n.d.

n.d.

2.42

n.d.

n.d.

n.d.

Sesquiterpenes
1

a-Cubebene

1345

1339

n.d.

0.11 0.01

0.03 0.01

0.05 0.01

Sativene

1394

1350

n.d.

0.07 0.01

n.d.

0.04 0.01

a-Ylangene

1370

1358

0.02 0.01

0.23 0.01

0.16 0.01

0.17 0.01

a-Copaene

1377

1362

n.d.

0.57 0.03

0.32 0.02

0.39 0.01

b-Bourbonene

1385

1368

0.03 0.01

n.d.

n.d.

n.d.

(Z)-b-Caryophyllene

1405

1391

n.d.

0.30 0.02

n.d.

0.22 0.01

(E)-b-Caryophyllene

1418

1404

n.d.

20.7 0.5

9.62 0.97

15.8 0.5

b-Copaene

1422

1416

n.d.

1.17 0.01

n.d.

n.d.

a-Bergamotene

1434

1432

n.d.

n.d.

0.41 0.03

n.d.

10

Humulene

1457

1445

n.d.

18.5 0.5

9.86 0.68

16.3 0.3

11

4,5-di-epi-Aristolochene

1467 (BP1)

1453

n.d.

0.10 0.01

n.d.

0.25 0.02

12

(E)-b-Famesene

1461

1459

n.d.

n.d.

1.07 0.12

0.75 0.01

13

c-Muurolene

1477

1466

0.01 0.01

1.27 0.02

n.d.

1.23 0.04

14

b-Selinene

1490

1471

n.d.

1.51 0.01

0.22 0.02

1.02 0.04

15

Eremophilene

1489

1473

n.d.

0.13 0.01

n.d.

0.08 0.01

16

a-Curcumene

1486

1475

0.02 0.01

n.d.

n.d.

n.d.

17

Gurjunene

1475

1476

n.d.

0.06 0.01

n.d.

0.06 0.01

18

a-Selinene

1498

1480

n.d.

1.59 0.02

0.19 0.01

1.03 0.03

19

c-Gurjunene

1473

1485

0.01 0.01

n.d.

n.d.

n.d.

20

b-Guaiene

1487

1487

n.d.

n.d.

0.03 0.01

0.08 0.01

21

a-Muurolene

1483

1489

0.01 0.01

0.24 0.01

0.17 0.01

0.19 0.01

22

c-Cadinene

1504

1499

n.d.

0.82 0.02

0.64 0.03

0.72 0.01

23

b-Bisabolene

1516

1500

n.d.

n.d.

0.05 0.01

n.d.

24

(E)-Calamenene

1505

1506

0.03 0.01

n.d.

0.09 0.01

0.10 0.01

25

(Z)-Calamenene

1520

1509

n.d.

0.11 0.01

0.13 0.01

0.11 0.01

26

d-Cadinene

1525

1512

n.d.

1.05 0.02

0.37 0.02

0.78 0.01

27

Cadinadiene-1,4

1539

1518

n.d.

0.13 0.01

0.07 0.01

0.10 0.01

28

a-Cadinene

1536

1523

n.d.

0.17 0.01

0.11 0.01

0.13 0.01

29

a-Calacorene

1542

1527

n.d.

0.05 0.01

n.d.

0.06 0.01

0.12

48.9

23.5

39.7

0.04 0.01

0.03 0.01

100

100

Sesquiterpenoids
1

Caryophyllene oxide

1582

1590

n.d.
100

n.d.
100

n.d., not detected; n.a., not available for HP5-MS or equivalent column. Retention indexes reported for the HP-5MS or equivalent column. Data mean of 3
replications
a

NIST [24]

123

784

Eur Food Res Technol (2013) 237:775786

Fig. 1 Spider plot showing the

main flavor parameters for 3 of
the herb liqueur samples (10
points scale 0 = none,
9 = extremely strong).
Significant differences were
found among these samples for
the flavors: sweet, bitter, mint,
chamomile, lemon verbena,
balsamic, herbal, and alcoholic
(p \ 0.05)

Fig. 2 Internal preference map showing overall liking for the herb liqueur samples. Samples: indicated in bold font. Filled circle NW-Spanish
consumers indicated with G; SE-Spanish consumers indicated with A

scale) liked significantly more than samples D, G, and E

(with scores close to 4 in a 9 points scale) (p \ 0.05). The
sample which received the highest punctuation was sample

123

B (90 % commercial ? 10 % Saaz liqueur), and the samples which received the lowest scores were the samples
with higher concentration of Nugget hop. Figure 2

Eur Food Res Technol (2013) 237:775786

785

Fig. 3 Partial least square map showing overall liking drivers for NW and SE-Spanish consumers. Sensory parameters indicated by the
descriptors in bold and italic font. Filled circle NW-Spanish consumers indicated with G; SE-Spanish consumers indicated with A

illustrates the internal preference map showing the overall

liking of consumers.
Also, significant differences (p \ 0.05) were found
when looking at sweetness, bitterness, and aromatic herbs
flavor liking. Again, the samples which were more liked for
the three parameters were the ones with Saaz hop liqueur
and also the commercial sample. If studying the JAR
questions for these attributes, the samples in which a higher
frequency of consumers answered JAR or the closest score
(456 in the 9 points JAR scale), were C and B (between
66 and 76 % of consumers marked 4, 5 or 6 for all these
parameter in these samples). Results seemed to indicate
that the commercial sample had a slight excess of sweetness that was not perceived in samples 706 and 153.
Regarding the JAR question about aromatic herb flavor,
76 % of respondents scored 46 in sample C (75 % commercial ? 25 % Saaz liqueur); therefore, the addition of a
small percentage of Saaz hop improved the perception of
this specific attribute. As expected, sample E (75 % commercial ? 25 % Nugget liqueur) was signaled as too
much flavor and too much bitterness for more than
50 % of consumers, and too slight sweetness for 34 % of
respondents.

Figure 3 shows a PLS map which illustrates the drivers

for consumers overall liking. As can be seeing in the map,
67 % of the total variation of the descriptive data explained
37 % of variation of overall liking. As shown in the figure,
consumers tend to like products which have higher intensities in aromatic herbs, lemon verbena, chamomile, and
mint flavors. Also, they liked high sweetness but, as shown
previously (JAR questions results), not in excess. In general, consumers liked structured and equilibrated products
which were perceived as unctuous as well. Results of the
present study showed that, contrary as expected, floral or
fruity flavors were not liking drivers, maybe because those
attributes were not associated with herb liqueurs but
with other kind of liqueurs such as limoncello (Italian
lemon liqueur) or similar fruit liqueurs.

Conclusions
Substantial differences were found when studying the suitability of Nugget and Saaz hop cultivars to make herb
liqueurs. Commercial liqueur with Nugget liqueur added
had a higher bitterness, astringency, pungency, herbaceous

123

786

Eur Food Res Technol (2013) 237:775786

notes, and also produced a higher alcoholic sensation

(p \ 0.05). Some of these attributes could be related to the
higher TPC of the Nugget liqueur sample, and also to the
fact that the volatile composition of both cultivars was pretty
different. In general, consumers did not like these herb
liqueurs made with Nugget hop. On the other hand, results
showed that the addition of fine aroma hops (Saaz) to make
herb liqueurs was appreciated by consumers, and maybe
liqueur companies should consider using this herb as a new
ingredient for their products. Adding Saaz hop increased the
liking of aromatic herbs flavor and also decreased the
perception of excess of sweetness for consumers. The
addition of this cultivar could bring new aromatic notes to a
product, giving to the liqueur unique characteristics. The
present study shows a useful example of how to evaluate the
suitability of an aromatic herb as ingredient to make a traditional product such as herb liqueur.
Acknowledgments Part of financial assistance for this project was
provided by the Ministry of Research and Science of Spain thought
the Juan de la Cierva subprogram. Also, we are grateful for the
financial support of this work to Diputacion de Ourense and University of Vigo (INOU12-15). In addition, the authors wish to thank
Jose Luis Olmedo Nadal, the company Hijos de Rivera Inversiones
Corporativas S.L., and the panelists of the Regulating Council of the
Geographical Denomination of the Spirits and Traditional Liqueurs
from Galicia for their kind collaboration in this particular study.
Conflict of interest

None.

7.

8.

9.

10.

11.

12.

13.
14.

15.

16.

Compliance with Ethics Requirements This article does not

contain any studies with human or animal subjects.
17.
18.

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