Eur Food Res Technol
DOI 10.1007/s00217-012-1775-y
ORIGINAL PAPER
Effect of maturation conditions on sensory and antioxidant
properties of old Serbian plum brandies
Sonja Pecić • M. Veljović • S. Despotović •
I. Leskošek-Čukalović • M. Jadranin •
V. Tešević • M. Nikšić • N. Nikićević
Received: 3 March 2012 / Revised: 19 June 2012 / Accepted: 25 June 2012
Ó Springer-Verlag 2012
Abstract Sˇljivovica and Prepecˇenica are traditional Ser-
bian distillated beverages made from varieties of plum, of
the genus Prunus. The ageing in wooden casks not only
improves the sensory characteristics, but also changes the
content of total polyphenols and contributes to the other
important health properties, such as the increase of their
antioxidant capacity. In this study, home-made brandy
(Sˇljivovica and Prepecˇenica) samples were used, which
matured in casks during the time period from 10 to
47 years. The aim of this investigation was to examine the
influence of the ageing parameters (time period and type of
wooden casks) and raw material (plum cultivars) on the
total polyphenol content, amount of certain phenol com-
pounds, sensory properties, colour and antioxidant prop-
erties in matured brandies. The individual phenol
components were determinated using HPLC system
equipped with diode array detector, while the total phenol
content and antioxidant activity was estimated using
spectrophotometric methods (Folin–Ciocalteu, DPPH,
FRAP and TEAC). Total polyphenol content (TPC) of aged
Prepecˇenica samples was ranged from 230.26 to
S. Pecić (&)  M. Veljović  S. Despotović 
I. Leskošek-Čukalović  M. Nikšić  N. Nikićević
Department of Food Technology and Biochemistry, Faculty of
Agriculture, University of Belgrade, Nemanjina 6, 11080
Zemun, Belgrade, Serbia
e-mail: pecic84@hotmail.com
M. Jadranin
Institutes for Chemistry, Technology and Metallurgy,
University of Belgrade, Njegoseva 12, 11000 Belgrade, Serbia
V. Tešević
Department for Instrumental Methods of Chemical Analysis,
Faculty of Chemistry, University of Belgrade, Studentski trg 16,
11000 Belgrade, Serbia
890.26 mg/L gallic acid equivalents (GAE mg/L), whereas
the TPC of Sˇljivovica sample was 110.38 mg/L. Antioxi-
dant capacity of analysed Prepecˇenica samples and
Sˇljivovica sample was in strong correlation with TPC. Total
sensory score of all samples was very high and varied
between 18.2 and 19.8. The obtained results have shown
that the benefit of longer maturation on sensory charac-
teristics is well recognized, but the improvement has some
limitation.
Keywords Plum brandy  Phenol compounds  Total
phenol content  Antioxidant capacity  Colour  Sensory
characteristics
Abbreviations
TPC Total polyphenol content
GAE Gallic acid equivalents
FRAP Ferric ion reducing antioxidant power
TE Trolox equivalent
TEAC Trolox equivalent antioxidant capacity
CU Colour units
Introduction
Slivovitz or Slivovitsa is a plum brandy primarily produced
in Slavic regions of Central and Eastern Europe such as
Czech Republic, Slovakia, Poland, Hungary and Bulgaria,
but most of all in Serbia as well known Sˇljivovica. It is the
most popularly consumed brandy in those nations, as well
as wherever communities of expatriate from these nations
exist. Similar plum brandies are also produced in Germany,
Switzerland, France, the United States and Canada, but
marketed under other names, such as brandy, Pflümli or
eau de vie.
123

Serbian Sˇljivovica is a brandy made of the distillates of
fermented plum fruit, variety Prunus domestica, with at
least 25 % (v/v) of ethanol content. Under the name of
Prepecˇenica has become known by double distillation,
with at least 40 % (v/v) of ethanol content [1].
Characteristic aromatic complex of plum brandy comes
from compounds, which can be classified into four groups
based on their origin: primary aromatic compounds—from
fruit raw material; secondary compounds—formed during
alcoholic fermentation; tertiary compounds—formed dur-
ing distillation process and quaternary compounds—
formed in casks during maturation process.
The basic aroma of Sˇljivovica and its most valuable
specificity arise from primary aromatic compounds, with
the largest quantity is in the inner layer of the plum skin.
Due to the great influence of these ingredients on the
characteristics and the quality of the final aroma, the plum
variety selection is of prime importance for the production
of a high-quality brandy. In Serbia, the most commonly
used plum types are follows: the autochthonous cultivars
(Crvena ranka, Metlaš), flavourful variety Požegača (ori-
gins from Malaysia) and the new types made by crossing
various plum species (such as Čačanska lepotica, Čačanska
rodna, Čačanska najbolja). Plum types with its distinctive
aromatic compounds give to the distillates the naturalness
and the characteristics of a local character [2].
The new distillates are not convenient for use due to
their inharmonious taste and sharp odour. Distillates have
to mature and undergo an ageing process in wooden casks.
The ageing in wooden casks is the most important step of
production process of several beverages (cognacs, whisky,
brandies, vinegars, calvados, mescal and wines). This
process not only improves the sensory characteristics, but
also changes the content of total polyphenols and develops
other important health properties, such as the increase of
their antioxidant capacity [3–9].
During the ageing process, plum distillates are harmo-
nized and the aromatic complex is encircled by quaternary
compounds, formed in complex chemical reactions. For the
ageing of plum distillates, mostly are used casks made of
two types of oak tree: Quercus peteraea L. (Q. sessiliflora)—
the Sessile Oak and Quercus pedunculata (Q. robur)—the
Pedunculate Oak. Much less frequently are used mulberry,
black locust, white ash, plum, cherry, elm and others casks,
due to their inferior contribution to the beverages quality.
Casks made of oak Quercus pedunculata, which grows in
the Kučaj mountains (eastern Serbia), are specially appre-
ciated in Serbia.
The wood tissue is mostly made of polysaccharides
(cellulose, hemicelluloses and lignin), which is impregnate
with tannins and small amount of lipids. The oak wood
contains only 10 % of organic components of dry sub-
stances that can be extracted [10]. Composition of the
123
Eur Food Res Technol
extract is very complex and depends on the tree species, its
origin and the single-tree effect [11].
The main extractive wood components are hydrolysable
tannins and volatile compounds [12]. Maturation is a very
complex process, based on a mixture of different reactions
between spirits (solution alcohol–water) and wooden cask,
which are in constant contact during the ageing process
[13]. The chemical compositions of spirits are, also,
changed during the ageing period. The concentration of
most polyphenols increases, but the increasing rate is not
constant during the years and it has a limitation point of
around 30 years, when the accumulation speed does not
change significantly [14].
On the other hand, in the last decade, the antioxidant
characteristics of beverages have become very important
quality. A lot of data have been published on wine and beer
properties and their antioxidant potentials. Increased sci-
entific research on the antioxidant capacity of many local
and commercial spirits, during recent years, has shown the
importance of this question as well.
The type of cask and the duration of maturation are two
variables, equally important for quality of old plum bran-
dies. Both parameters of ageing process in production of
whisky and cognac are defined according to the interna-
tional or local regulation for the product name [15].
According to the Serbian tradition, brandy has been kept
for several decades in different wooden casks, but the local
regulation for Serbian brandies does not define the ageing
parameters. They depend, a lot, on the local production
practice.
The aim of this study was to examine the influence of
the ageing parameters (time period and type of wooden
casks) on the total polyphenol content, content of phenol
compounds, colour and antioxidant characteristic in
matured plum brandies. Additionally, the influence of raw
material (different plum cultivar) and the ageing parame-
ters on the sensory characteristics of Prepecˇenica samples
and Sˇljivovica sample were specified.
Materials and methods
Chemicals
Gallic acid (GA), Folin–Ciocalteu’s phenol reagent,
hydrochloric acid, sodium acetate trihydrate, glacial acetic
acid and sodium carbonate were purchased from Merck
(Darmstadt, Germany). 2,4,6-Trypyridyl-s-triazine (TPTZ),
ferric chloride hexahydrate, 2,2-diphenyl-1-picrylhydrazyl
(DPPH), 6-hydroxy-2,5,7,8-tetramethylchroman-2-carbo-
xylic acid (Trolox), sodium dihydrogen phosphate, sodium
hydrogen phosphate, sodium chloride, 2,20 -azinobis (3-
ethylbenzothiazoline-6-sulphonic acid) diammonium salt
Eur Food Res Technol
(ABTS), potassium persulfate were purchased from Sigma-
Aldrich (Steinheim, Germany). Standards of gallic acid,
4-hydroxy benzaldehyde, vanillic acid, syringic acid,
vanilin, syringaldehyde, ferulic acid, coniferaldehyde,
sinapaldehyde and ellagic acid were purchased from
Sigma–Aldrich (St. Louis, MO, USA). All the chemicals
were HPLC grade. Ultra high-purified water, methanol
HPLC grade and formic acid from Merck (Darmstadt,
Germany) were used as solvent for chromatography.
Samples
Home-made brandy (Sˇljivovica and Prepecˇenica) samples,
which matured in casks in the time period from 10 to
47 years, have been used in this study. All samples were
made from traditional plum varieties of the genus Prunus,
which are used to obtain high-quality brandy in local
households. The study has included 9 samples of Prep-
ecˇenica and one Sˇljivovica sample:
S1. Prepecˇenica (44.8 % (v/v)) made of a plum variety
called Požegača, originated from the Goč Mountain; the
distillate was left to mature in a cask made of species
Quercus petreae L. from 2000.
S2. Prepecˇenica (45 % (v/v)) made of a variety called
Požegača, distilled twice in 1990, left to mature in an
oak cask, species Quercus petreae L.
S3. Prepecˇenica (45 % (v/v)) made of a variety called
Požegača, distilled twice in 1978, left to mature in an
oak cask, species Quercus petreae L.
S4. Prepecˇenica (43 % (v/v)) made of a plum variety
called Crvena ranka, distilled twice in 1976, left to
mature in an oak cask, species Quercus petreae L.
S5. Prepecˇenica (42 % (v/v)) made of a plum variety
called Požegača, distilled in 1970, left to mature in an
oak cask, species Quercus pedunculata for 10 years, and
then kept in an oak cask coated with paraffin.
S6. Prepecˇenica (44 % (v/v)) made of a plum variety
called Požegača, distilled twice in 1994, left to mature in
an oak cask, species Quercus pedunculata.
S7. Prepecˇenica (46 % (v/v)) made of a plum variety
called Požegača, distilled twice in 1990, left to mature in
an oak cask, species Quercus pedunculata until 2008,
and then stored in glass barrels.
S8. Prepecˇenica (44.3 % (v/v)) made of an autochtho-
nous plum variety called Metlaš, distilled twice in 1988,
left to mature in an oak cask, species Quercus petreae L.
(oak from the Kučaj Mountain) until 2005, and then
stored in glass barrels.
S9. Prepecˇenica (45 % (v/v)) made of an autochthonous
plum variety called Bugarka (variety of Crvena ranka),
distilled twice in 1989, left to mature in a mulberry cask
until 2007, and then stored in glass barrels.
S10. Sˇljivovica (28 % (v/v)) made of a plum variety
called Crvena ranka, distilled twice in 1955, left to
mature in an oak cask, species Quercus pedunculata
until 1985, and then stored in glass barrels.
Determination of total polyphenols
Determination of the TPC in brandy samples has been
conducted by the Folin–Ciocalteau method described by
Singleton and Rossi [16].
Briefly, 2.5 ml of Folin–Ciocalteu’s solution (diluted
with distilled water in 9:1 ratio) was added to the diluted
samples (0.1 mL sample ? 0.4 mL 96 % (v/v) ethanol),
agitated to homogenize and left to stand in the dark for
5 min in order to perform reaction. Two millilitres of
Na2CO3 solution (75 g/L) were added and left for 2 h in
the dark; absorbance was measured at 760 nm. The cali-
bration curve was prepared with GA solution, and the
results were expressed as GAE/L. All the measurements
were performed in triplicate.
DPPH radical scavenging activity
For the determination of antioxidative characteristics of
samples, the DPPH was used, Ferric ion Reducing Anti-
oxidant Power (FRAP) and Trolox Equivalent Antioxidant
Capacity (TEAC) method.
DPPH-reducing activity was evaluated following the
modified procedure described by Kaneda, Kobayashi,
Furusho, Sahara and Koshino [17]. Brandy samples
(0.2 mL) (diluted in different ratio with 96 % (v/v) etha-
nol) were added to the DPPH working solution (2.8 mL)
(mixture of 0.186 9 10-4 mmol/L DPPH in ethanol and
0.1 M acetate buffer (pH 4.3) in ratio 2:1). The absorbance
at 525 nm was measured after 90 min of incubation in the
dark. DPPH reagent and distilled water were used as a
blank reference. The Trolox calibration curve was plotted
as a function of the inhibition percentage of DPPH radical.
The results were expressed as mM of Trolox equivalents
per litre of brandy. The percentage of DPPH inhibition was
calculated by following formula: Activity [ % of DPPH
reduction] = [A - As/A] 9 100 %, where A—absorbance
of DPPH solution with ethanol and As—absorbance of a
DPPH solution with sample.
All experiments were performed in triplicate.
FRAP assay
FRAP assay was performed according to the procedure by
Benzie and Strain [18]. FRAP reagent solution was made
of the mixture of acetate buffering agent (pH = 3.6), TPTZ
(10 mM solution TPTZ in 40 mM HCl) and FeCl3 9 6H2O
123

in volume ratio 10:1:1, respectively). All samples, stan-
dards and reagents were pre-incubated at 37 °C. An aliquot
of each diluted brandy sample (0.1 mL) was mixed with
3 mL of FRAP reagent. After the reaction at 37 °C for
40 min, the absorbance at 593 nm was measured. The
standard curve was constructed by using serial dilution of
Trolox stock solution (1 mM). The FRAP value was
obtained by using following equation:
FRAP ¼ mM Trolox equivalents  2
TEAC assay
The TEAC assay was conducted according to the pro-
cedure described by Re et al. [19], with some modifi-
cations. A solution of 14 mM of ABTS and 4.9 mM
potassium persulfate was prepared in a phosphate buffer
(pH 7.4) and mixed in equal volumes to produce a stable
ABTS*? stock solution. The obtained dark blue-green
stock solution was left in the dark at room temperature
for 12–16 h before use. A working ABTS*? solution was
prepared by diluting ABTS*? stock solution (approxi-
mately 1/80 dilution) to an absorbance of 0.70 ± 0.02
absorbance units (AU) at 734 nm and 30 °C using
phosphate buffer. After addition of 3.0 mL of working
ABTS*? solution to 30 lL of brandy samples or Trolox
standards (2.5, 1.25, 0.625, 0.3125 and 0.15625 mM
Trolox solutions in phosphate buffer), the absorbance
reading was taken at 30 °C, 6 min after initial mixing.
Appropriate solvent blanks were run in each assay. The
fractional inhibition (FI) of ABTS*? radical was calcu-
lated and plotted as dose–response (DR) curves (i.e.,
concentration vs. fractional inhibition) for Trolox and
each sample. The TEAC value was calculated using the
following equation:
TEAC ðmMTEÞ ¼ ðGradient of sample DR curve=
 Gradient of Trolox DR curveÞ:
Liquid chromatographic analysis of phenolic
compounds
Samples were filtered through a 0.45-lm pore size mem-
brane filter before injection. An Agilent 1100 HPLC sys-
tem (Agilent Technologies, Palo Alto CA-USA) operated
by Windows NT-based ChemStation software was used.
The HPLC equipment was used with a diode array detector
(DAD). System consisted of a binary pump, degasser and
auto sampler. The column used was a Lichrospher 100
RP18 (4.0 mm 9 250 mm, 5 lm). The mobile phase
consisted of two solvents: Solvent A. water/formic acid
(96:4; v/v) and Solvent B. methanol (100 v/v). Phenolic
compounds were eluted under the following conditions:
1 mL min-1 flow rate and the temperature was set at 40 °C
123
Eur Food Res Technol
gradient programme (0–3.0 min. 0 % B; 3.0–25 min.
0–28 % B; 25–43 min. 28–42 % B; 43–55 min. 42 % B;
55–60 min. 42–56 % B; 60–65 min. 56 % B; 65–66 min.
56 % B; 66–70 min. 0 % B) followed by washing and
reconditioning the column. The ultraviolet–visible spectra
(scanning from 190 to 450 nm) were recorded for all peaks.
Triplicate analyses were performed for each sample. The
identification of phenolic compounds were obtained out by
comparing the retention times and ultraviolet–visible
spectra with authentic standards, while quantification was
performed by external calibration with standards.
Colour determination
Colour determinations of distillate beverages were deter-
mined according to the AOAC method [20]. The standard
curve was made with solutions of K2Cr2O7 (0.05 - 0.5 g/
L) in 0.005 M H2SO4, whose absorbance was determined
at 430 nm and expressed in colour units (CU), ranges from
1 to 10.
CIELab chromatic parameters
Colour measurements were made on brandy samples using
a portable trismulus colour analyser Chomametar model
CR410. Results were expressed in Commission Interna-
tionale d Eclairage L*, a* and b* colour—space co-ordi-
nate. These parameters defined L* (lightness), a*(from
green to red), b* (from blue to yellow), C* (chroma or
saturation) and h (hue angle). CIElab parameters were
calculated for the CIE illuminant D65.
Sensory analysis
Sensory analysis was performed by modified Buxbaum
model of positive ranking with maximum 20 points [21].
The points were distributed by following characteristics:
clearness—parameter, which contributes to the overall
visual liking of beverage; it depends on the purity and hue
of colour (max 1 points); colour—visual impression cre-
ated as a result of irritation of the retina of the eye with
light rays of different wavelengths (max 1 points); dis-
tinction—parameter, which clearly defines specific and
distinctive characteristic synonymous for certain categories
of strong alcoholic beverages (max 2 points); odour—a
sensory attribute, resulting from stimulation of the olfac-
tory receptors in the nasal cavity by certain volatile sub-
stances (max 6 points); taste—a sensory attribute, resulting
from stimulation of the gustatory receptors in the oral
cavity by certain soluble substances (max 10 points) [22].
The analysis was conducted by evaluation panel, made of 5
sensory experts. All evaluation experts had long tradition in
evaluation of alcohol beverages. Samples were diluted with
Eur Food Res Technol

Table 1 Total polyphenol content (TPC) and antioxidant characteristic of plum brandy
Samples of old Ageing period Wood species of TPC FRAP TEAC DPPH
plum brandy (years) cask (mg GAE/L)a (FRAP units) (mM TE)b (mM TE)b

S1 11 Sessile oak 230.26 ± 2.83a 1.99 ± 0.08a 1.49 ± 0.03a 1.05 ± 0.02a
b a b
S2 21 Sessile oak 280.90 ± 4.04 2.82 ± 0.07 1.98 ± 0.02 1.29 ± 0.01b
b b c
S3 33 Sessile oak 292.69 ± 3.85 6.78 ± 0.41 4.14 ± 0.04 2.33 ± 0.09c
c b d
S4 35 Sessile oak 408.08 ± 0.38 6.16 ± 0.43 5.28 ± 0.06 2.30 ± 0.03c
b b c
S5 41 (10)* Pedunculate 284.87 ± 10.69 6.26 ± 0.36 4.54 ± 0.03 1.94 ± 0.03d
c c e
S6 17 Pedunculate 434.23 ± 5.00 8.67 ± 0.44 3.51 ± 0.02 2.91 ± 0.07e
S7 50 (47)* Pedunculate 480.51 ± 15.00d 8.00 ± 0.30c 6.09 ± 0.02f 2.78 ± 0.06e
S8 23 (17)* The Kučaj’s oak 890.26 ± 34.62e 19.35 ± 0.46d 8.89 ± 0.02g 6.43 ± 0.01f
S9 22 (18)* Mulberry 275.38 ± 2.31b 1.99 ± 0.08a 3.50 ± 0.02e 1.05 ± 0.01a
f e h
S10 56 (30)* Pedunculate 110.38 ± 3.53 0.87 ± 0.12 0.71 ± 0.02 0.50 ± 0.02g
Different letters in same row denote a significant difference according Tukey’s test, at p \ 0,01
For definitions of samples S1 to S10, refer the text under the section ‘‘Samples’’
* Number in bracket defines the years of storing in wooden cask
a
Total phenol content, expressed as milligram of Gallic acid equivalents per litre of brandy
b
Total antioxidant capacity expressed as mmol of Trolox equivalent

distilled water to reach an alcohol proof of 40° (% v/v),
except the sample 10, which had an alcohol proof of 28°
(% v/v).
Statistical analysis
All measurements were done in triplicate, and data were
expressed as mean ± standard deviation (SD). The exper-
imental data were subjected to a one-way analysis of var-
iance (ANOVA), and Tukey’s test was calculated to detect
difference (p B 0.01) between the mean values. Statistical
analyses were performed with the statistical program MS
Excel (Microsoft Office 2007 Professional). The correla-
tion coefficient between antioxidant activity and total
phenol content, also between total phenol content and
colour, was determined by using MS Excel (Microsoft
Office 2007 Professional).
Results and discussion
The TPC and the antioxidant capacity are shown in
Table 1. In our study, TPC of aged Prepecˇenica samples
were ranged from 230.26 to 890.26 mg GAE/L, whereas
the TPC of Sˇljivovica sample was 110.38.
Gorjanović et al. [23] estimated the amount of total
polyphenol content and the antioxidant activity in the plum
brandy stored in an oak cask (during 5 years of maturation
process) and inox steel (stainless steel) tank. They showed
that the brandy, left to mature in an oak cask (for 5 years),
had significantly higher amount of polyphenolic com-
pounds (153 mg GAE/L) and antioxidant capacity,
compared with the brandy that was stored in inox tank
(8.4 mg GAE/L).
The time of maturation and the botanic species of
wooden casks show significant influence on TP content of
aged brandies [3, 23]. TP content of brandy samples
matured in Pedunculate oak casks shows higher values
than Sessile oak wood which is in correlation with pre-
viously result [3, 15, 24, 25]. During the ageing in oak
cask, the content of polyphenols increased, but the rate
of accumulation was not constant. The results have
shown that the sample S8, aged in the Kučaj’s oak cask
(Q. robur), originated from eastern Serbia, had the highest
TPC. The mulberry wood is sometimes used to replace
common oak wood. TP content is higher than Sessile oak
and smaller than Pedunculate oak for the same ageing
period. According to the obtained results, Sˇljivovica
sample (S10) (28 % (v/v)) had the smallest content of
TPC. Based on these facts, we can conclude that the
content of alcohol is extremely important for extracted
wood components.
Many different assays are used for the measurement of
antioxidant capacity, since there is no standardized method.
Three methods (FRAP, TEAC, DPPH) were selected to
analyse and compare the results of these measurements.
Antioxidant capacity of analysed samples is strongly
correlated with TP content (Table 2), with the highest
correlation (R2 = 0.952) between TPC and DPPH method.
Considering that the antioxidant in the brandy comes from
wooden cask, the chemical composition and wood variety
are very important for TPC and antioxidant characteristic.
The results of quantitative determination of several low-
molecular-weight phenolic compounds were present in

123
 Eur Food Res Technol

71.3 ± 5.37b

36.3 ± 1.27d

2.45 ± 0.35g
14.45 ± 0.92a
16.75 ± 0.78a

19.25 ± 0.21a
27.8 ± 0.42c

93.8 ± 0.42e
3.70 ± 0.53f
Table 2 Correlation between TPC and antioxidant characteristics

38.35 ± 1.2d
Ellagic acid
R2 TPC FRAP TEAC DPPH

TPC 0.922 0.825 0.952

FRAP 0.807 0.992

Sinap aldehyde

1.05 ± 0.06bc
TEAC 0.802

b
0.77 ± 0.13a

a
0.51 ± 0.03

0.35 ± 0.05

0.73 ± 0.06
nd

nd
nd

nd
nd
Table 2. During maturation, the concentration of phenols
was increased due to decomposing of the insoluble com-

Coniferyl aldehyde
ponent of wooden casks. The phenols, such as vanillin,

a,b,f

a,e,f
d

a,e
syringaldehyde, vanillic acid, syringic acid, coniferalde-

1.43 ± 0.08b
b

3.97 ± 0.09g
h

d
1.63 ± 0.11a

1.05 ± 0.06c
1.94 ± 0.06

2.14 ± 0.05
1.84 ± 0.05
0.73 ± 0.06

0.65 ± 0.09
1.32 ± 0.03
hyde, ferulic acid, 4-hydroxy benzaldehyde and sinapal-
dehyde, are the degradation products of lignin. The content
of ellagitannins and gallotannins was decreasing during
the year of maturation through the hydrolysis with forma-

d
5.57 ± 0.11a

1.25 ± 0.07f
5.00 ± 0.04
4.12 ± 0.04
2.04 ± 0.05
Ferulic acid
tion of ellagic acid and gallic acid, respectively [26]
(Table 3).

nd
nd

nd

nd
nd
The botanical species of wood had a larger influence on
the phenols composition of spirits than time of maturation,

Syring aldehyde
but the time of maturation strongly affected on the amount

Different letters in same row denote a significant difference according Tukey’s test, at p \ 0,01; refer as in Table 1
g
b

5.46 ± 0.11b

d
5.24 ± 0.13a

9.30 ± 0.06e
f
4.72 ± 0.05

4.46 ± 0.14
7.36 ± 0.15
8.68 ± 0.03
7.62 ± 0.08

1.46 ± 0.09
3.84 ± 0.16
of these compounds. The main contributors of antioxidant
power of samples were the phenolic acids, including ella-
gic, gallic and vanillic acid [3]. The ellagic acid was the
most abundant component in all brandy samples. The

2.36 ± 0.07b

b
4.17 ± 0.07a
a

4.66 ± 0.13c
content of ellagic acid in samples maturated in sessile and

f
4.36 ± 0.02

3.05 ± 0.05
4.81 ± 0.04
5.01 ± 0.02
3.76 ± 0.14

1.70 ± 0.04
2.59 ± 0.22
pedunculate oak is higher than content of gallic acid.
Vanillin

Increased level of these acids with the time of maturation

was detected in all samples maturated in oak’s cask
(S1 \ S2 \ S3 and S5 \ S6). However, the extension of

h
Syringic acid

d
1.67 ± 0.02a

7.44 ± 0.07c
a

a
f
2.76 ± 0.07

2.91 ± 0.10
6.68 ± 0.18
9.81 ± 0.11
6.22 ± 0.12
7.08 ± 0.08
0.06 ± 0.01
2.81 ± 0.15
ageing time in wooden casks over a certain time (approx-
imately 33–35 years) resulted in a significant reduction of
gallic and ellagic acid content (S4 \ S3 and S7 \ S6).
Also, the content of compounds such as vanillin,
ab

ab
2.82 ± 0.07b

syringaldehyde, vanillic acid, syringic acid, coniferalde-

2.33 ± 0.12a
a

6.12 ± 0.10e
Vanillic acid

g
2.14 ± 0.06

2.28 ± 0.12
3.82 ± 0.08
5.27 ± 0.08
2.26 ± 0.07

1.34 ± 0.07
Table 3 Phenolic compounds in the old Serbian brandy samples

1.77 ± 0.1
hyde and sinapaldehyde which originated from lignin was
increasing during the time, but the amount of these com-
pounds was significantly decreased in the samples older
than 33 year. It can be concluded that the process of lignin
4-Hydroxy benzaldehyde

decomposition was finished after 33 year. The sinapalde-

hyde was not detected in the sample S3, S5 and S8.
0.71 ± 0.02a,c,d

In casks production, the mulberry wood is sometimes

cd

a,b
b

d
0.61 ± 0.06a
a

0.63 ± 0.03a

e
0.62 ± 0.02

0.45 ± 0.02
0.83 ± 0.06
0.94 ± 0.01
0.52 ± 0.01

0.77 ± 0.02
0.24 ± 0.01

used to replace common oak wood. The sample (S9)

maturated in mulberry wood had the lower content of
polyphenol then other samples, and it is interesting that
only in this sample of Prepecˇenica, gallic acid was not
b

27.35 ± 0.11h
1.24 ± 0.08a

13.40 ± 0.16c

detected.
3.56 ± 0.11

2.13 ± 0.05
5.30 ± 0.02
18.09 ± 0.12
7.51 ± 0.16
Gallic acid

Alcohol strength of brandy significantly influences

extraction of wood components [27]. The Šljivovica sam-
nd
nd

ple with 28 % v/v of ethanol had very low quantity of

phenol components. Based on the results, the most abun-
Sample

dant phenol component in Šljivovica were syringaldehyde

S10
S1
S2
S3
S4
S5
S6
S7
S8
S9

and syringic acid. The gallic acid was not detected, and the

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Eur Food Res Technol

1000
R² = 0.845
800

TPC (mg GAE/L)

600

400

200

0
0 10 20 30 40
Colour (CU)

Fig. 2 Relation between total phenol content and colour (colour unit)
for plum brandies

Fig. 1 Colour of plum brandies, expressed in colour unit. Refer as in
Table 1
content of ellagic acid was significantly lower than in
Prepečenica sample.
The sample S8 matured in Kučaj oak had the highest
content of phenol components and the highest value of
antioxidant capacity. This sample had the highest amount
of gallic acid, vanillic acid, syringaldehyde, coniferyl
aldehyde, sinapaldehyde and ellagic acid compared with
other analysed samples. According to these results, the
Kučaj’s oak is the best material for the wooden cask
production.
Colour measurement
After distillation, plum brandies are colourless, and during
the ageing process, the colour changes in different tones
from yellow to brown. The part of extracted polyphenol
from wood is decomposed by the action of atmospheric
oxygen, which results with colour changing and reduction
of astringency [3]. The aged brandy colour is very com-
plex, and it is difficult to describe it and compare. To solve
this problem, the spectroscopy method was used for
the determination colour of whisky (Fig. 1), which also
depends on the content of extracted ingredients during
ageing process in wooden casks.
Sample S8 shows significantly higher value for colour
(34.93 CU, p \ 0.01) than other samples of plum brandies,
matured in an oak cask. The colour of this sample is very
rare for the plum Prepecˇenica, and the sensory expert
described it as a flame of mahogany colour with shades of
purple cognac as background colour. This specific colour
comes from a magnificent oak wood, which originates from
the Kučaj mountains. We observed that the alcohol content
had influence on the colour degree as well.
Strong correlation (R2 = 0.845) was determined
between TPC and the colour (Fig. 2). With increasing
polyphenol content, the colour of aged brandy became
more intensive.
CIElab method was used for more specific and more
objective determination of colour (Table 4). The value of
lightness (L*) was decreased during the period of matu-
ration and with extraction of polyphenols. It was obvious
that the content of polyphenols had significant influence on
the lightness of analysed samples. The value of parameter
a* was in range from 0.16 to 16.94, while the parameter b*
was from 21.17 to 35.16. Based on hue angle, a* and b*
values, it can be concluded that colour of all samples was
yellow, with certain proportion of red colour. Brandy

Table 4 CIELab chromatic

Sample L*(D65) a*(D65) b*(D65) C*(D65) h (D65)
parameters of plum brandy
samples S1 40.98 ± 0.01 6.32 ± 0.01 31.01 ± 0.01 31.65 ± 0.01 78.48 ± 0.03
S2 36.28 ± 0.01 6.11 ± 0.01 25.42 ± 0.01 26.15 ± 0.01 76.48 ± 0.01
S3 36.18 ± 0.01 13.55 ± 0.03 30.19 ± 0.04 33.09 ± 0.02 65.83 ± 0.07
S4 37.84 ± 0.01 6.34 ± 0.03 27.73 ± 0.03 28.47 ± 0.02 77.14 ± 0.07
S5 46.86 ± 0.01 2.21 ± 0.02 31.32 ± 0.01 31.40 ± 0.01 85.96 ± 0.03
S6 36.41 ± 0.01 9.68 ± 0.03 29.00 ± 0.02 30.57 ± 0.02 71.54 ± 0.07
S7 41.22 ± 0.01 10.49 ± 0.03 35.76 ± 0.01 37.27 ± 0.00 73.65 ± 0.06
S8 36.19 ± 0.02 16.94 ± 0.05 31.29 ± 0.04 35.58 ± 0.05 61.57 ± 0.07
S9 38.76 ± 0.01 10.74 ± 0.03 31.82 ± 0.02 33.58 ± 0.02 71.36 ± 0.05
S10 49.14 ± 0.01 0.16 ± 0.01 21.17 ± 0.01 21.17 ± 0.00 89.56 ± 0.02
Refer as in Table 1

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Table 5 Sensory analysis of

Plum brandy Assessment characteristic
maturated plum brandies
samples
Colour Clearness Distinction Odour Taste Total
(max 1 pts) (max 1 pts) (max 2 pts) (max 6 pts) (max 10 pts) (max 20 pts)

S1 1 1 2 5.6 ± 0.1 9.1 ± 0.1 18.7 ± 0.2

S2 1 1 2 5.8 ± 0.2 9.9 ± 0.2 19.7 ± 0.1
S3 1 1 2 5.8 ± 0.1 9.8 ± 0.1 19.6 ± 0.2
S4 1 1 2 5.9 ± 0.2 9.9 ± 0.1 19.8 ± 0.1
S5 1 1 2 5.6 ± 0.1 8.6 ± 0.1 18.2 ± 0.2
S6 1 1 2 5.9 ± 0.2 9.8 ± 0.1 19.7 ± 0.2
S7 1 1 2 5.7 ± 0.2 9.4 ± 0.1 19.1 ± 0.3
Each number is presented as S8 1 1 2 5.7 ± 0.2 9.0 ± 0.2 18.7 ± 0.2
mean ± SD of five evaluations
S9 1 1 2 5.8 ± 0.2 9.5 ± 0.2 19.2 ± 0.2
of sensory experts
S10 1 1 2 5.7 ± 0.2 9.1 ± 0.1 18.8 ± 0.1
Refer as in Table 1

Table 6 The results of statistical analyses with total score of the Požegača, which was left to mature in a wooden cask for
sensory evaluation 10 years and then kept in inox cask. The part of the sensory
S1 S2 S3 S4 S5 S6 S7 S8 S9 S10 component evaporated and decomposed, which reduced the
influence on the sensory impression of sensory experts. It is
S1 – – ** ** ** ** ** ** ** – interesting that the sensory value of sample S8 with the
S2 – ** ** ** ** ** ** ** – highest TPC was high, but significantly lower than other
S3 ** ** ** ** ** ** ** – sensory evaluated samples. This sample is made of a plum
S4 – ** ** – – – ** cultivar called Metlaš, which partly influences the taste
S5 – ** – – – ** and has lower value for this assessment characteristic.
S6 – – – – ** According to the results, it is established that the sample
S7 – – – ** made of a plum cultivar called Crvena ranka had the best
S8 – – ** evaluated taste characteristic, and based on this result, we
S9 – ** suggest that this plum cultivar should be used for the
S10 ** production of the highest quality plum brandy. Based on
Tukey’s test (p \ 0.01) was applied to the comparative analysis of the
our investigation, characteristics of wooden casks do not
total score of the sensory evaluation of plum Prepečenica have significant influence on the sensory characteristics of
** shows very significant different values the samples matured during the period from 11 to 47 years.
– not significant The content of ethanol has strong influence on mouth
feel and taste of spirits [21]. The Sˇljivovica sample (S10)
with 28 % (v/v) alcohol had one of the lowest taste values,
maturated in Kučaj’s oak had the lowest value for hue which is in accordance with the previous statement.
angle and L*, and the highest value for a*, which indicates For the sensory characteristic, the influence of plum
that this sample had the highest proportion of red colour. variety plays an important role, especially on the taste, but
Hue angle of Šljivovica (S10) was 89.56, which means that it is obvious that the overall score was affected by various
this sample was almost completely yellow. other factors.

Sensory evaluation
The sensory evaluation of plum brandies is presented in
Table 5. The results of one-way ANOVA (F = 6.30,
p = 0.00) indicate that difference between samples was
statistically very significant (Table 6). Total sensory score
of all samples was very high and varied between 18.2 and
19.8. The best evaluated sample (19.8) was sample S4
made of a plum variety called Crvena ranka, left to mature
for 33 years in the sessile oak wooden cask. The lowest
score (18.2) had sample S5, made of a plum variety called
Conclusion
Maturation process, significantly, influences the content of
polyphenols and antioxidant capacity of aged plum bran-
dies. On the basis of these results, Kučaj oak species,
Quercus petreae L., is the material proposed for the pro-
duction of casks used for maturation of Sˇljivovica, but the
chemical composition of this wood material will be further
investigated. The obtained results have shown that the
benefit of longer maturation on the sensory characteristic

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Eur Food Res Technol
is well recognized, but the improvement has limitation. The
results suggested that the extended maturation (after
35 years) seemed to have no further affect.
Acknowledgments This work was supported by the Ministry of
Education and Sciences of Serbia grants no. 46001/172053.
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