food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950

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Food and Bioproducts Processing

journal homepage: www.elsevier.com/locate/fbp

Effect of spray drying on the physicochemical

properties and color stability of the powdered
pigment obtained from vinication byproducts of
the Bordo grape (Vitis labrusca)

Volnei Brito de Souza , Marcelo Thomazini, Julio Csar de Carvalho Balieiro,

Carmen Slvia Fvaro-Trindade
Universidade de So Paulo, Faculdade de Zootecnia e Engenharia de Alimentos (FZEA/USP), Avenida Duque de
Caxias Norte, 225, CEP: 13635-900, Pirassununga, So Paulo, Brazil

a b s t r a c t

The aim of this work was to produce and evaluate powdered pigments obtained from vinication byproducts of
Bordo red grapes (Vitis labrusca). The concentrated extract obtained from the byproducts was spray dried under
different conditions of inlet air temperatures (130170 C) and carrier concentration (1030%) in a total of 9 treatments.
Besides, one sample of freeze-dried extract was obtained to comparison. The samples were analyzed by: moisture
content, anthocyanin retention, hygroscopicity, water solubility, moisture sorption isotherms, infrared spectroscopy
(FTIR), and changes in color during storage. Moisture content and anthocyanin retention were inuenced by the
drying temperature and carrier agent concentration, whereas hygroscopicity was more inuenced by the carrier
concentration. The moisture sorption isotherms were also inuenced by the maltodextrin concentration. Infrared
spectroscopy indicated that the extract was covered or encapsulated by the carrier agent. During storage, samples
containing maltodextrin preserved the color more intensely than the freeze-dried sample and the liquid extract.
Results suggested that spray drying of Bordo grape extracts using maltodextrin produces powders with low moisture
content, low hygroscopicity, high solubility, and stable color. These results evidence that this byproduct of wine
production may be used as a natural source of pigments.
2013 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Keywords: Pomace; Anthocyanins; Atomization; Sorption isotherms; Color parameters; Encapsulation

1. Introduction Shrikhande, 2000; Llobera and Canellas, 2007; Rockenbach

Grapes are one of the most commonly cultured fruits all
over the world (Xu et al., 2010). Among American grapes
(Vitis labrusca), Bordo cultivar is one of the most used in
South America, mainly in the production of wines and
juices (Rizzon et al., 2000; Pozzan et al., 2012). Grape
processing generates a large amount of byproducts, mainly
peels and seeds, corresponding to about 20% of the weight
of the processed grape. These byproducts may be consid-
ered interesting sources of anthocyanins, and may be used
in the production of natural pigments (Bagchi et al., 2000;
et al., 2011).
Anthocyanins are one class of the avonoid compounds,
and are the most important pigments of vascular plants. They
are innocuous and easily incorporated into aqueous media,
making them interesting options to be used as water-soluble
colorants (Giusti and Wrolstad, 2003). However, the stability of
these molecules may be affected by several factors, such as pH,
storage temperature, light, oxygen, solvents, metal ions, etc.
Therefore, the study of anthocyanin stabilization has been the
main focus of recent studies due to their high potential for use
and their benecial effects (Castaneda-Ovando et al., 2009).

Corresponding author. Tel.: +55 19 3565 4282; fax: +55 19 3565 4284.
E-mail addresses: volnei@usp.br, volnei15@gmail.com (V.B. de Souza).
Received 10 June 2013; Received in revised form 30 October 2013; Accepted 4 November 2013
Available online 11 November 2013
0960-3085/$ see front matter 2013 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.fbp.2013.11.001
40 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950
Table 1 pH, soluble solids ( Brix), total anthocyanin content and composition of concentrated liquid extract (% wet
basis) obtained from Bordo grape byproducts.
Parameter Mean standard deviation
pH
Soluble solids
Acidity
Moisture
Carbohydrates
Fats
Ashes
Proteins
Fibers
Total anthocyanins (mg/g of extract dry basis)
a
Not measurable.
Spray drying is a continuous, simple and fast process in
which a liquid or paste is transformed in a powdered dry prod-
uct after a relatively short drying period. The process involves
the atomization of the liquid in a compartment that receives
a ow of hot air. Quick evaporation of the water keeps the
temperature of the particles low. Therefore, this technique
enables drying of heat-sensitive products (food, biological,
and pharmaceutical products), without affecting their qual-
ity too much (R, 1998). However, fruit juice powders obtained
by spray drying have some inconvenient properties, such as
high stickiness, high hygroscopicity, and low solubility, mak-
ing their storage and use considerably difcult (Cano-Chauca
et al., 2005).
Carrier agents have been used to overcome these problems,
with maltodextrin as one of the most common ones (Cano-
Chauca et al., 2005; Ahmed et al., 2010; Tonon et al., 2010; Berg
et al., 2012), mainly because of its high solubility and low vis-
cosity which are important characteristics in spray drying
(Tonon et al., 2010).
Drying conditions, such as drying air temperature and con-
centration of the carrier agent, among others, may inuence
different characteristics of the nal material (Tonon et al.,
2008; Comunian et al., 2011; Fazaeli et al., 2012; Ferrari et al.,
2012; Frascareli et al., 2012). Therefore, it is interesting to study
the inuence of these conditions in the characteristics of the
product, as well as in its properties and stability.
Valduga et al. (2008) studied the extraction and spray dry-
ing of anthocyanins of the pulp of Isabel grapes (V. labrusca).
However, these authors carried out a study on the extraction
and drying process, analyzing only the responses total antho-
cyanin content and color parameters. The present trial was a
deeper study of the responses to the spray drying process with
grapes of a different variety. The following analyses were car-
ried out in the powders: sorption isotherms, FTIR, and color
stability during storage, which were not carried out in the
study cited above. Rockenbach et al. (2011) studied extracts of
different grape varieties, among them the Bordo (V. labrusca),
and analyzed anthocyanin and phenolic content, as well as
antioxidant activity. However, Rockenbach et al. (2011) ana-
lyzed liquid extracts, and did not obtain powdered pigments,
as it was done in the present study.
Therefore, the objectives of the present study were to pro-
duce powdered pigments of byproducts (seeds and peels) from
Bordo grape (V. labrusca) by extraction and spray drying using
maltodextrin as the carrier agent, in order to evaluate the
effect of the drying conditions on the properties of the powder
and color stability during storage.
Analytical method
3.43 0.01 Potentiometer
5.33 0.06 Refractometer
2.95 0.01 AOAC (2006)
95.67 0.32 AOAC (2006)
0.80 0.01 AOAC (2006)
0.17 0.01 AOAC (2006)
0.41 0.06 AOAC (2006)
NMa AOAC (2006)
NMa AOAC (2006)
102.30 1.77 Giusti and Wrolstad (2001)
2. Materials and methods
2.1. Materials
Byproducts (seeds and peels) of Bordo red grapes (V. labrusca)
from wine production were used, which were provided by Vin-
cola Micheletto, located in the city of Louveira, So Paulo,
Brazil. The pomace was packed under vacuum in a semi-
automatic packing machine (model 200S, Selovac, So Paulo,
Brazil) using a low density polyethylene lm, and were stored
in a freezer at 20 C. The carrier agent used in the atomization
process was maltodextrin MOR-REX 1910 (9 DE 12, called
here 10-DE), kindly provided by Ingredion (Mogi-Guacu, Brazil).
2.2. Production of liquid extracts
Grape peels and seeds were thawed at refrigeration tempera-
ture (4 C) for 12 h. The solvent used was 67.6% (v/v) aqueous
ethanol. Ethanol concentration was determined in a prelim-
inary assay. The proportion of pomace:solvent was 1:3 (w/v)
(Terci and Rossi, 2002). The mixture solventpomace was
ground in a blender (model RI 2008, Walita, Varginha, Brazil),
and extraction was performed under mechanical stirring (stir-
rer model 713, Fisaton, So Paulo, Brazil) for 3 hours at room
temperature and away from light (Valduga et al., 2008). The
mixture was ltered in a cotton cloth, and the ethanol extract
was stored at 20 C.
Before concentration, the extract was centrifuged (model
5810R, Eppendorf, Hamburg, Germany) at 3000 rpm for 5 min.
Then, it was concentrated in a rotary evaporator (TE-211, Tec-
nal, Piracicaba, Brazil) at 60 C, until it was reduced to 1/3 of
the initial volume. The concentrated liquid extract was char-
acterized in relation to the concentration of lipids, total sugar,
moisture, ashes, bers, protein, and acidity. The physical char-
acteristics evaluated were pH, measured in a potentiometer
(model MB-10, Marte, Piracicaba, Brazil), and soluble solids,
measured in a portable digital refractometer (model AR200,
Reichert, Depew, USA). The parameters analyzed in the extract
are presented in Table 1.
2.3. Spray drying
The mixture extract-maltodextrin was homogenized manu-
ally. Spray drying was carried out in a pilot spray dryer (model
MSD 5.0, Labmaq do Brasil Ltda, Ribeiro Preto, Brazil) that
used a 2 mm nozzle and air ow of 40 L/min. The compres-
sor air pressure was 0.2 MPa and the feed rate of the mixture
 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950 41

Table 2 Outlet temperature and responses to the experiments in the spray dryer, of extracts obtained from vinication
byproducts of Bordo grape under different temperatures and carrier concentration. The responses to freeze-dried sample
without carrier agent also are showed.
Treatment Inlet air Carrier agent Moisture Anthocyanin Hygroscopicity Solubility Outlet
temperature concentration content retention (%)a (g water/100 g (%)a temperature
( C) (%) (%)a dry matter)a ( C)a

1 130 10 4.39 0.17 93.87 0.45 16.04 0.16 91.84 1.91 91.50 2.12
2 130 20 4.40 0.01 95.88 1.21 13.76 0.07 95.29 0.30 93.50 3.54
3 130 30 4.54 0.07 93.04 1.17 12.44 0.48 94.40 0.77 93.00 1.41
4 150 10 3.35 0.14 88.36 0.07 16.27 0.22 94.93 0.04 111.50 0.71
5 150 20 3.29 0.02 92.49 1.88 14.53 0.31 96.66 0.32 117.00 1.41
6 150 30 3.90 0.02 94.25 0.95 13.35 0.32 97.20 0.43 106.50 2.12
7 170 10 2.96 0.02 90.83 0.29 16.90 0.41 95.29 0.02 116.00 0.00
8 170 20 3.50 0.10 94.04 0.14 14.29 0.33 97.49 0.25 121.00 0.00
9 170 30 3.72 0.01 97.35 1.82 14.54 0.43 96.97 1.31 128.00 1.41
Freeze-dried 1.02 0.12 52.56 0.53 17.42 0.68 74.41 0.83
extract

a
Mean standard deviation.

was 44 mL/min, performed by a peristaltic pump. A 3 3 fac-
torial arrangement in a completely randomized design (CRD)
was used, and variables tested were inlet air temperature (130,
150, and 170 C) and concentration of the carrier (10, 20, and
30% expressed with respect to the total mass of concentrated
extract), in 9 treatments (Table 2) with two repetitions, total-
ing 18 assays. Responses evaluated were moisture content,
anthocyanin retention, hygroscopicity, and solubility of the
samples.
2.4. Freeze-dried control
A sample of freeze-dried extract was prepared to be used for
comparison. The concentrated extract was frozen at 20 C
and freeze-dried in the proper equipment (model LC 1500,
Terroni, So Carlos, Brazil) for 24 h. The sample obtained was
stored at 20 C.
2.5. Moisture content
Moisture content of the powders was determined in a mois-
ture analyzer (MB35 Halogen, Ohaus, Switzerland) using
infrared radiation and a halogen heating lamp.
2.6. Total anthocyanin content
Total anthocyanin content was determined by pH differen-
tial method (Giusti and Wrolstad, 2001). Absorbance was read
at 520 and 700 nm. Results were expressed (in dry basis)
as monomeric anthocyanin content (mg/g) of malvidin-3-
glucoside equivalents. Molecular extinction coefcient used
was 28,000 L/cm mol, and molecular weight of 463.3 g/mol
(Rockenbach et al., 2011). For anthocyanin retention, total con-
tent was determined in the mixture or extract before the
atomization or freeze-drying process, as well as in the prod-
ucts obtained.
means of the mass of water adsorbed by the sample, and was
expressed in g of adsorbed water/100 g of dry matter.
2.8. Solubility
Solubility was determined using the method by Eastman and
Moore (1984), with some modications. The method consisted
in the addition of 0.5 g of sample in a container with 50 mL of
distilled water and stirring at 100 rpm in an orbital table (model
TE-420, TECNAL, Piracicaba, Brazil) for 30 min, followed by cen-
trifugation at 3000 rpm for 5 min. Later on, a 25 mL aliquot of
the supernatant was removed and placed in an incubator at
105 C until its weight was constant. Solubility was calculated
based on the initial mass of the sample that was solubilized in
the 25 mL aliquot of the supernatant. The result was expressed
as a percentage.
2.9. Sorption isotherms
The equilibrium moisture of the powdered samples were
determined by the static gravimetric method (Labuza, 1984),
with some modications. Initial moisture of the samples was
measured, and then weighted and stored for 3 weeks at
25 C, in desiccators containing salt solutions with relative
humidities ranging from 31.3% to 90.9% measured in Aqualab
(Decagon Devices, Pullman, WA, USA). Moisture content was
calculated by means of the weight gain, and experimental
equilibrium moisture content was determined by means of
the ratio between the total mass of water and the dry mass of
the sample. Experimental data were adjusted to the GAB and
modied BET models, according to Eqs. (1) and (2), respectively.
Xm CGAB KGAB aw
Meq = (1)
(1 KGAB aw ) (1 KGAB aw + CGAB KGAB aw )
N N+1
Xm CBET aw [1 (N + 1) (aw ) + N (aw ) ]
Meq = N+1
(2)
(1 aw ) [1 (CBET ) aw CBET (aw ) ]

2.7. Hygroscopicity where Meq is the equilibrium moisture content (g water/100 g

Hygroscopicity analysis was carried out according to Cai and
Corke (2000), with some modications. Triplicates of 0.5 g
aliquots of each sample were placed in Petri dishes and, later
on, stored for one week in a desiccator containing NaCl sat-
urated solution (RH 75.3%). Hygroscopicity was measured by
dry matter); Xm is the moisture in the molecular monolayer (g
water/100 g dry matter); aw is the water activity; N is the num-
ber of molecular layers; and CGAB , KGAB , CBET are the constants
of the respective models.
Isotherms were modeled according to the equations using
the Solver tool in Microsoft Excel (Microsoft, Redmond,
42 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950
USA). Criteria of choice for the best adjustments were the
determination coefcient (R2 ), and the module of the relative
average deviation (RD), calculated according to Eq. (3).
100  |EV PV|
RD = (3)
n EV
where EV = experimental value; PV = value predicted by the
model; n = number of observations.
2.10. Fourier-transformed infrared spectroscopy (FTIR)
The spectra for pure maltodextrin, pure water, concentrated
extract, freeze-dried extract, and samples after spray drying
were obtained in the 4000600 cm1 range using a Perkin Elmer
spectrometer Spectrum One (Massachusetts, USA) and the
Spectrum One software version 5.3.1.
2.11. Color stability
The methodology described by Tonon et al. (2010) was used,
with some adaptations. Small amounts of the samples were
placed in containers for maximum surface exposure. After
that, samples were stored in desiccators containing MgCl2
saturated solution (RU 32.8%). Desiccators were stored in incu-
bators at 25 C. Samples were stored for 120 days in these
conditions, and analyzed every 30 days for color parameters.
Color parameters were measures in a colorimeter (model Mini
Scan XE, HunterLab, Reston, USA), and results were expressed
according to the CIELAB color system (L*, a*, and b*). Calibration
was done using black and a white calibration plates.
2.12. Statistical analysis
In order to evaluate the effect of the treatments (inlet
temperature and carrier concentration) on moisture con-
tent, anthocyanin retention, hygroscopicity, and solubility of
the spray-dried samples, the analysis of variance was used
(p < 0.05), and regression analysis was used to evaluate the
interaction between the factors, in which the inuence of one
factor (inlet temperature or carrier concentration) was ana-
lyzed for each level of the other factor. When there was no
interaction, the main effects of each factor were analyzed sep-
arately.
The analysis of variance (p < 0.05) and Tukeys range test
(p < 0.05) were used to assess signicant differences between
the samples in the color stability test. All statistical tests were
carried out in the SAS statistical package (Statistical Analysis
System), version 9.2.
3. Results and discussion
Atomization produced uid powders of purple color, with hue
variation according to the concentration of the carrier agent.
The freeze-drying process yielded an almost black sample that
clumped easily.
3.1. Responses to the drying study
Responses to the treatments in relation to moisture content,
anthocyanin retention, hygroscopicity, and solubility, as well
as outlet air temperature are presented in Table 2.
Outlet temperature has a better correlation with quality
of spray dried product (Anandharamakrishnan et al., 2007).
However, in this work was used the inlet temperature as vari-
able of process because it can be controlled in the equipment.
Outlet air temperatures presented in Table 2 are values pro-
vided by the equipment and showed variation even for equal
values of inlet air temperature.
3.2. Moisture content of the powders
The moisture content of the spray dried samples was inu-
enced both by drying air temperature and concentration of
the carrier agent (Fig. 1).
Increased carrier concentration (Fig. 1a) yielded con-
stant moisture content in the samples at the lowest drying
temperature, and increased moisture content in the other
temperatures. This result can be explained by the higher
viscosity of the feeds with higher concentration of maltodex-
trin that reduced the heat and mass transfer, reducing the
evaporation of water. Tonon et al. (2008) did not observe any
inuence of the concentration of the carrier agent in the mois-
ture content of spray dried acai juice. Fazaeli et al. (2012)
observed a decrease in moisture content with increased car-
rier concentrations in mulberry juice spray dried with different
concentrations of maltodextrin.
Decreased moisture content was observed with the
increase in drying air temperature (Fig. 1b). This was due to
the high temperatures used, which led to greater energy trans-
ferred to the mixture, and evaporation of greater amounts of
water. This result was similar to the one reported by Goula
and Adamopoulos (2005), for spray dried tomato pulp; Maury
et al. (2005), for spray dried trehalose; Tonon et al. (2008), for
acai juice spray dried with maltodextrin; Silva et al. (2013), for
dried jabuticaba peel extracts using maltodextrin as the car-
rier agent; and Fazaeli et al. (2012), for spray dried mulberry
juice with maltodextrin.
Moisture contents in the present study ranged from 2.96%
to 4.94%. Similar results were reported by Moreira et al. (2009),
for acerola pulp extracts spray dried with different percent-
ages of carrier agents, which showed moisture content ranging
from 3.09% to 5.43%; and Silva et al. (2013), who reported mois-
ture contents ranging from 2.11% to 5.31%, in jabuticaba peel
extracts spray dried with maltodextrin as the carrier agent.
Moisture content of the freeze-dried sample was lower than
that of the spray dried samples (Table 2). However, the freeze-
drying process takes much more time (24 h) to reach the same
moisture content of atomized samples, in which drying is
almost immediate. Besides, the spary-dried product without
the carrier is difcult to be handled, preventing its use.
3.3. Anthocyanin retention
Both drying air temperature and concentration of the carrier
agent signicantly inuenced anthocyanin retention in atom-
ized samples (Fig. 2).
It may be observed, in Fig. 2a, that with increased mal-
todextrin concentrations, anthocyanin retention was constant
at the lowest temperature. However, there was an increase
in retention when higher temperatures were employed. This
increased retention may be explained by non-enzymatic
browning, specically caramelization of the carrier agent.
Caramelization yields dark compounds that are quantied
in the total anthocyanin content. Another kind of reaction
that may explain this result is linked to the presence of
proanthocyanidins in the sample, which mainly come from
the grape seeds in the residue. According to Schwartz et al.
 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950 43

5 5
a) b)
4.5 4.5

Moisture content (%)

Moisture content (%)

4 4

3.5 3.5

3 3

2.5 2.5

2 2
10 12 14 16 18 20 22 24 26 28 30 130 135 140 145 150 155 160 165 170
Maltodextrin (%) Temperature (C)

Fig. 1 Moisture content on the spray-dried samples of Bordo grape extracts: (a) According to the temperature (,
Y130 C = 4.45; . . .. . ., Y150 C = 4.06 0.10M + 0.003M2 ; ------, Y170 C = 2.63 + 0.04M). (b) According to the carrier agent
concentration (, Y10% = 8.96 0.04T; . . .. . ., Y20% = 43.53 0.51 T + 0.002T2 ; ------, Y30% = 19.90 + 0.19T + 0.001T2 ). Where ,
, , are the observed mean of the combinations temperature-concentration of maltodextrin (N = 2) and bars refer to the
respective standard errors; M = maltodextrin concentration; T = inlet air temperature.

(2010), although colorless, proanthocyanidins or condensed samples dried at 180 C, compared with those dried at 160 and
tannins may be converted to colored anthocyanidins during 200 C. They concluded that in systems containing maltodex-
processing, mainly when there are acids and high tempera- trin of low DE, drying air temperatures may reach 180 C. Silva
tures are used. The increase in anthocyanin retention could et al. (2013), who dried jabuticaba peel extracts with maltodex-
also be attributed to the better protection achieved when trin at temperatures of 140, 160, and 180 C, observed greater
higher carrier agent concentrations were used. anthocyanin retention at 160 C, a temperature closer to the
Fig. 2b shows that, with increased temperature and less highest one used in the present study (170 C).
carrier agent (10%), there was a decrease in anthocyanin reten- High anthocyanin retention was observed in the present
tion due to the degradation of these molecules, followed by a study, ranging from 88.36% to 97.35%. Retention observed in
small increase that may have been caused by non-enzymatic atomized samples was greater than that of the lyophilized
browning and degradation of proanthocyanidins. When 20% sample (Table 2). The length of exposure of the sample during
of carrier was used, retention remained constant with the the freeze-drying process, which is much longer than that of
increase in temperature; and when 30% maltodextrin was the atomization process, contributes to anthocyanin degrada-
used, retention increased. The fact that samples containing tion. High values of anthocyanin retention were also reported
greater percentages of the carrier did not show decreased by Silva et al. (2013), ranging from 83.21% to 99.02% for jabu-
retention may indicate both a protective effect of the car- ticaba extract atomized at different temperatures and using
rier agent, and the occurrence of more intense caramelization maltodextrin as the carrier agent.
and degradation of proanthocyanidins. Tonon et al. (2008)
observed a decrease in anthocyanin retention in acai juice 3.4. Hygroscopicity
with increased drying temperatures. Ersus and Yurdagel (2007)
also found loss of anthocyanins with increased entry air tem- The concentration of the carrier agent was the factor that most
perature in the atomization of black carrots using three types inuenced hygroscopicity in atomized samples (Fig. 3).
of maltodextrin as carrier agents. However, these last authors There was a decrease in hygroscopicity in samples with
did not nd differences in anthocyanin content with varia- greater contents of the carrier agent, as shown in Fig. 3a. How-
tions in drying air temperature when maltodextrin 10-DE was ever, for samples dried in the highest temperature (170 C),
used, with even a small increase in anthocyanin content in there was an increase in hygroscopicity when maltodextrin

100 100
a) b)
98 98
Anthocyanin retention (%)

Anthocyanin retention (%)

96 96
94 94
92 92
90 90
88 88
86 86
84 84
82 82
10 12 14 16 18 20 22 24 26 28 30 130 135 140 145 150 155 160 165 170
Maltodextrin (%) Temperature (C)

Fig. 2 Anthocyanin retention on the spray-dried samples of Bordo grape extracts: (a) According to the temperature (,
Y130 C = 94.26; . . .. . ., Y150 C = 85.82 + 0.29M; ------, Y170 C = 87.55 + 0.33M). (b) According to the carrier agent concentration
(, Y10% = 323.74 3.06T + 0.01T2 ; . . .. . ., Y20% = 94.14; ------, Y30% = 78.70 + 0.11T). Where , , , are the observed mean of
the combinations temperature-concentration of maltodextrin (N = 2) and bars refer to the respective standard errors;
M = maltodextrin concentration; T = inlet air temperature.
44 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950

18 18
a)

Higroscopicity (g water/100g dry matter)

b)

Higroscopicity (g water/100g dry matter)

17 17
16 16
15 15
14 14
13 13
12 12
11 11
10 10
10 12 14 16 18 20 22 24 26 28 30 130 135 140 145 150 155 160 165 170
Maltodextrin (%) Temperature (C)

Fig. 3 Hygroscopicity on the spray-dried samples of Bordo grape extracts: (a) According to the temperature (,
Y130 C = 17.69 0.18M; . . .. . ., Y150 C = 17.64 0.15M; ------, Y170 C = 22.380.69 M + 0.014M2 ). (b) According to the carrier agent
concentration (, Y10% = 16.41; . . .. . ., Y20% = 14.19; ------, Y30% = 5.55 + 0.05T). Where , , , are the observed mean of the
combinations temperature-concentration of maltodextrin (N = 2) and bars refer to the respective standard errors;
M = maltodextrin concentration; T = inlet air temperature.

concentration changed from 20% to 30%. More porous or due to the production of more porous particles when higher
fragmented particles are produced at higher temperatures, temperatures are used in the drying process.
increasing the surface of the particles exposed to the humid- Besides, hygroscopicity of atomized samples was signif-
ity (data related to particles morphology not shown). Decrease icantly lower than that of the lyophilized sample without
in hygroscopicity is related with characteristics of the car- the carrier agent (Table 2). This result emphasizes that the
rier agent. Maltodextrin 10-DE is one of the most commonly presence of the carrier agent contributes to the decrease in
used materials in spray drying because of its low hygroscopic- hygroscopicity of grape dried extract.
ity, among other characteristics. Similar results were reported
by Tonon et al. (2008), who found lower hygroscopicity val- 3.5. Solubility
ues with increased concentrations of maltodextrin. The same
authors found hygroscopicity values ranging from 12.48 to There was no signicant variation in the solubility of the sam-
15.79 g of water/100 g of dry matter, results that are very close ple, either with the variation in temperature or maltodextrin
to the ones found in this study, which ranged from 12.44 concentration. However, solubility was greater when com-
to 16.90 g of water/100 g of dry matter. Cai and Corke (2000), pared with the lyophilized sample without the presence of the
when drying amaranth betacyanins, also observed that mal- carrier agent (Table 2). The presence of maltodextrin increases
todextrin may help to reduce hygroscopicity, reinforcing the the solubility of atomized samples due to this carrier that is
potential use of this material as a carrier agent. Comunian highly soluble in water, making it one of the main materi-
et al. (2011) spray dried chlorophyllide using maltodextrin and als used in spray drying (Cano-Chauca et al., 2005; Grabowski
other carriers and came to the conclusion that hygroscopic- et al., 2006; Goula and Adamopoulos, 2010).
ity was reduced with increased concentrations of the carrier High solubility found in this study, ranging from 91.84%
agent. to 97.49%, with an average of 95.57%, were also observed by
With the increase in temperature (Fig. 3b), only samples Cano-Chauca et al. (2005) who reported solubility above 90%
dried with greater percentages of the carrier agent (30%) pre- for spray dried powdered mango using maltodextrin as the
sented signicant increase in hygroscopicity, which may be carrier agent.

Table 3 Adjustment parameters to the moisture sorption isotherms in the samples of atomized Bordo grape extracts
stored at 25 C.
Model Parameters Samplea

1 2 3 4 5 6 7 8 9

GAB Xm (% b.s) 7.786 7.343 5.610 10.612 5.724 4.135 10.428 6.750 3.997
CGAB 0.534 1.487 1.484 2.414 0.808 0.577 0.982 2.280 0.684
K 0.752 0.946 0.967 0.939 0.907 0.836 0.864 0.975 0.899
R2 0.974 0.983 0.971 0.998 0.992 0.980 0.997 0.996 0.984
RD% 8.658 8.205 9.258 4.397 7.757 9.447 3.838 5.790 9.527

BET Xm (% b.s) 4.613 3.856 3.582 4.737 4.172 4.189 4.516 3.623 3.535
CBET 6.845 3.308 1.687 3.781 1.953 1.097 1.359 2.570 1.723
N 32.268 30.508 31.251 28.288 24.969 21.042 25.911 39.511 26.153
R2 0.979 0.985 0.975 0.998 0.993 0.983 0.990 0.997 0.987
RD% 3.164 6.385 9.091 2.470 6.202 8.570 5.054 4.446 7.691

Where Xm is the moisture in the molecular monolayer (g water/100 g dry matter); aw is the water activity; N is the number of molecular layers;
and CGAB , KGAB , CBET are the constants of the respective models.
a
Samples: see Table 2.
 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950 45

Fig. 4 Moisture sorption isotherms of powdered Bordo grape extracts, dried under different temperatures and carrier
concentration: (a) adjust to GAB model; (b) adjust to BET model. Samples: see Table 2.

3.6. Sorption isotherms
Adjustment parameters of the experimental data to models
GAB and BET are presented in Table 3. Adjustments show high
R2 and relative average deviation lower than 10%. Moisture of
the molecular monolayer (Xm ) presented in these models is an
important parameter. It corresponds to the amount of water
strongly adsorbed to specic sites on the surface of the mate-
rial. It is considered a critical value, above which degradation
reactions are easier and the stability of the material is reduced
(Gabas et al., 2007; Tonon et al., 2009; Reid and Fennema, 2010;
Rocha-Selmi et al., 2013). Values for Xm ranged from 3.53%
to 4.17% in the BET model, and from 4.00% to 10.61% in the
GAB model. It was also observed that the moisture in the
monolayer decreased as the percentage of the carrier agent
increased, which is explained by Gabas et al. (2007) where, the
presence of the maltodextrin and gum Arabic probably modify
the balance between hydrophilic/hydrophobic sites, promot-
ing greater sorption of water. Silva et al. (2006) observed that
the addition of 30% maltodextrin 20-DE in camu-camu pulp
reduced Xm from 15.8% to 6.5% (in dry basis).
As for KGAB , it may be observed (Table 3) that it is inside the
range proposed by Lewicki (1997), based on the mathemat-
ical analysis of the model, from 0.24 K 1. Values of KGAB ,
46 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950
Fig. 5 Infrared spectra of ingredients, freeze-dried sample, and atomized samples of Bordo grape extracts. Samples: see
Table 2.
the correction factor for the properties of the molecules in the
multilayer related to the volume of the liquid, ranged from
0.752 to 0.975. KGAB below 1 is characteristic of food prod-
ucts (Rocha-Selmi et al., 2013). As for the sorption constant
C, which is related to interactions between active sites of the
product and water molecules, values below 200 were observed
in the two models, values that are inside the range described
in the literature (Alexandre et al., 2007; Pavn-Garca et al.,
2011; Rocha-Selmi et al., 2013).
Sorption isotherms adjusted to the spray-dried samples by
the GAB and BET models are presented in Fig. 4. All samples
showed a type III sorption isotherm, which was described by
Brunauer et al. (1938). The same prole was observed by Gabas
et al. (2007), Tonon et al. (2009), and Comunian et al. (2011) for
pineapple pulp, acai juice, and chlorophyllide, respectively, all
of which were spray dried using different carriers, including
maltodextrin.
3.7. FTIR analysis
Infrared spectra of the ingredients, freeze-dried extract, and
spray-dried samples are presented in Fig. 5.
Pure maltodextrin spectrum presented peaks of 1153, 1080,
and 1015 cm1 . The peaks of 1153 and 1080 cm1 are caused
by stretching of the C O bond, and the 1015 cm1 peak to the
angular deformation of the CH and CH2 bonds, all from
groups found in the carbohydrates (Socrates, 2001; Krishnaiah
et al., 2012).
The large band found from 2800 to 3700 cm1 in samples
of concentrated extract, freeze-dried extract, and in samples
atomized in lower intensity, is related to hydrogen bonds, and
stretching of the O H bond of carbohydrates, carboxylic acids,
and residual water (Coates, 2000; Socrates, 2001; He et al.,
2007). The spectrum related to pure water corroborates this
fact. In the spray-dried and freeze-dried samples, this band
is less intense than in the liquid extract due to the mois-
ture removed in the drying process. The liquid extract shows
this band, similar to pure water, once it has about 96% mois-
ture. Double peaks, near 2900 cm1 , more pronounced in the
freeze-dried sample, almost imperceptible in the concentrated
extract, and less intense in spray-dried samples, are produced
by the asymmetric and symmetric stretching of the C H bond
of the methyl group (Coates, 2000).
The 1641 cm1 band found in the water and liquid extract is
due to the angular deformation of H O H, indicating the pres-
ence of water or residual water in atomized and lyophilized
samples. The hydrogen bonds of the OH groups of carbohy-
drates may also contribute to this band (He et al., 2007). This
result may explain the variation in this band that was observed
between the samples of freeze-dried and atomized extracts.
 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950 47

Table 4 Color parameters L* (luminosity), a* (difference between red and green) and b* (difference between blue and
yellow) to the atomized samples, freeze-dried extract and concentrated liquid extract from Bordo grape during storage at
25 C and 32.8% relative humidity.
Treatment Day 0 30 days 60 days 90 days 120 days

Parameter L*
1 24.75 0.31E,a 24.38 0.9C,a,b 23.30 0.6C,a,b 22.75 0.7C,b 21.76 0.7C,b
2 30.76 0.2C,D,a 31.36 0.40B,a 30.49 0.27B,a 31.11 0.61B,a 31.00 0.34B,a
3 35.30 0.55A,a 36.37 0.52A,a 37.06 0.62A,a 36.09 0.24A,a 35.66 0.81A,a
4 23.45 0.39F,a 21.99 0.3C,D,b,c 23.24 0.4C,a,b 19.56 0.07D,d 21.08 0.4C,c
5 29.56 0.19D,b 30.86 0.34B,a 30.79 0.27B,a 30.20 0.30B,a,b 30.40 0.31B,a,b
6 32.61 1.10B,C,a 35.63 0.29A,a 35.90 1.21A,a 35.08 0.21A,a 35.70 1.01A,a
7 24.40 0.14E,F,a 21.67 1.21D,b 22.15 0.2C,a,b 21.39 0.0C,b 21.29 0.5C,b
8 30.13 0.28D,b 32.18 0.09B,a 31.34 0.35B,a,b 31.27 0.66B,a,b 31.02 0.00B,a,b
9 33.08 0.93B,a 36.12 1.56A,a 35.57 0.89A,a 36.24 0.29A,a 35.88 1.50A,a
Freeze-dried extract 8.13 0.08G,a 0.69 0.04E,c 1.04 0.16D,b 0.54 0.02F,c 0.63 0.02D,c
Liquid extract 1.36 0.30H,b 1.03 0.04E,b 2.05 0.05D,a 2.45 0.08E,a 2.13 0.09D,a

Parameter a*
1 27.61 0.25A,B,a 27.95 0.11B,a 28.30 0.54B,a 28.08 0.32A,B,a 27.41 0.43D,a
2 27.82 0.18A,b 29.47 0.08A,a 29.44 0.17A,a 28.87 0.24 A,a 28.97 0.08A,B,a
3 27.32 0.03A,B,b 28.53 0.41A,B,a 28.86 0.24A,B,a 28.52 0.16 A,a 28.50 0.11A,B,C,a
4 27.84 0.11A,b 29.51 0.43A,a 28.82 0.19A,B,a 26.46 0.0C,D,c 27.63 0.2C,D,b
5 27.29 0.37A,B,b 29.37 0.05A,a 29.32 0.20 A,a 28.96 0.37 A,a 29.24 0.03A,a
6 26.99 0.19B,b 28.57 0.14A,B,a 28.30 0.00 B,a 28.43 0.35 A,a 28.53 0.00A,B,C,a
7 27.57 0.03A,B,a 27.83 0.62B,a 28.46 0.04 B,a 27.18 0.28 B,C,a 27.22 0.45D,a
8 27.00 0.05B,b 28.38 0.06A,B,a 28.24 0.31 B,a 28.02 0.24 A,B,a 27.99 0.15B,C,D,a
9 24.86 0.2C,b 26.27 0.1C,a 25.90 0.0 C,a 25.99 0.29 D,a 25.76 0.07E,a
Freeze-dried extract 2.08 0.04E,a 1.70 0.33E,a,b 0.76 0.10 E,c 0.92 0.22 F,b,c 0.14 0.20G,c
Liquid extract 3.29 0.27D,d 3.57 0.12D,c,d 4.62 0.01 D,c 5.91 0.45 E,b 7.81 0.47F,a

Parameter b*
1 7.33 0.0C,c 5.83 0.2C,b 5.24 0.0C,a,b 5.41 0.24D,a,b 4.73 0.2C,a
2 9.08 0.05E,b 7.89 0.15D,E,a 7.72 0.23D,a 7.62 0.17E,a 7.47 0.08D,a
3 9.67 0.02 F,G,b 8.77 0.03E,F,G,a 8.81 0.13F,a 8.62 0.09F,a 8.61 0.06F,a
4 7.79 0.0C,e 7.50 0.05D,d 5.51 0.0C,c 4.51 0.0C,a 4.73 0.0C,b
5 9.61 0.03F,b 8.04 0.18D,E,F,a 7.87 0.15D,a 7.80 0.10 E,a 8.09 0.09D,E,F,a
6 10.17 0.12G,H,b 9.03 0.20G,a 8.66 0.17E,F,a 8.66 0.05 F,a 8.62 0.19F,a
7 8.50 0.10D,c 5.72 0.1C,b 5.55 0.0C,a,b 5.09 0.14 D,a 5.33 0.1C,a,b
8 10.40 0.08H,c 8.28 0.13D,E,F,G,b 8.19 0.04D,E,a,b 8.05 0.11 E,a,b 7.80 0.16D,E,a
9 10.61 0.03H,b 8.83 0.10F,G,a 8.69 0.10E,F,a 8.71 0.14F,a 8.42 0.18E,F,a
Freeze-dried extract 0.81 0.39A,a 1.20 0.59B,a 0.27 0.10B,a 0.05 0.02B,a 0.30 0.40B,a
Liquid extract 1.09 0.02A,B,d 0.58 0.17A,c 1.32 0.18A,b 2.41 0.13A,a 2.91 0.03A,a

Mean standard deviation. Equal Small letters in the same row and equal capital letters in the same column to each parameter do not differ
statistically by Tukeys test (p < 0.05). Treatment: see Table 2.

Generally, in the region between 1680 and 900 cm1 , sev-
eral bands from phenolic compounds found in grapes may be
observed. The bands of 16001520 cm1 may be assigned to
the vibration of the C C bond, typical of aromatic systems
(Edelmann et al., 2001).
Peaks around 13081212 cm1 are related with the pres-
ence of condensed tannins (proanthocyanidins) (Laghi et al.,
2011; Ping et al., 2012). These peaks may be mainly seen in
freeze-dried extract, and less intensely, in atomized samples.
Proanthocyanidins are mainly found in grape seeds, which
were part of the byproducts used.
Organic acids and sugars present one or more alcohol
groups (OH), having C O and O H bonds. C O bond show
peaks at the 10601150 cm1 range, indicating the presence
of these compounds (Fragoso et al., 2011). In fact, two peaks
around this band were observed in the spectra of pure mal-
todextrin and in samples dried with this carrier. The presence
of these two peaks in atomized samples and their absence in
the freeze-dried extract indicates that the extract was covered
by maltodextrin in the spray drying process.
Other peaks found in the samples, between 900 and
1100 cm1 , which may be assigned to valence vibrations of the
C O bond, and stretching vibrations of the C O C bond of
carbohydrates, such as glucose (Fragoso et al., 2011), which is
found in maltodextrin. The 1021 cm1 peak found in the atom-
ized samples, for example, may also have been affected by the
presence of the carrier.
In general, it may be observed that spray drying did not lead
to the formation of new bonds between maltodextrin and the
components of the extract, once similar peaks were observed
in the ingredients and atomized samples. The more intense
peaks in the spray-dried samples mainly result from acids and
sugars found in the extract added to the sugars of the carrier
agent. The intensity of the peaks of the samples were variable
and depended, for example, on the residual moisture and con-
centration of the carrier agent, leading to the dilution of the
compounds in the extract and decreasing the intensity of the
peaks.
3.8. Color changes during storage
Table 4 shows the variation in color parameters, L*, a*, and
b*, during the storage period at 25 C and 32.8% of relative
48 food and bioproducts processing 9 3 ( 2 0 1 5 ) 3950
humidity in samples that were atomized, freeze-dried without
carrier, and in the concentrated liquid extract.
The comparison between the atomized samples showed
that the most different parameter was luminosity, L*. Samples
dried with the greatest concentration of the carrier agent were
lighter, showing greater values of luminosity. As the carrier
is white, greater percentages of this material makes samples
lighter, and values obtained for the parameter L* are higher.
Besides, the sample dried at the lowest temperature (130 C)
was the lightest of all. This sample was probably the one less
susceptible to caramelization. This result indicates that drying
temperature also inuenced this parameter. Similar results
were reported by Tonon et al. (2009) in spray dried acai juice
using maltodextrin 10-DE as the carrier agent. Among all sam-
ples, the darkest one was the freeze-dried extract, showing
the lowest L* value, probably because it was the most concen-
trated sample, with the lowest moisture content, and did not
have maltodextrin.
During storage, parameter b*, which measures the differ-
ence between blue () and yellow (+), was the most affected
one. It was observed that samples presented an increase in
this parameter during the storage period, indicating loss in
blue color caused by anthocyanin degradation, the pigments
responsible for this color. The monomeric anthocyanin found
in greater amounts in red grapes is malvidin-3-glucoside
(Amico et al., 2004; Luque-Rodrguez et al., 2007; Rockenbach
et al., 2011). According to Schwartz et al. (2010) malvidin is the
anthocyanidin more important for the blue color. Idham et al.
(2012) also observed an increase in the parameter b* in antho-
cyanins during the storage period. However, they attributed
this result to the fact that samples became brown with time
because of the increase in the yellow color (increase in b*).
In some cases, there is a decrease in parameter a*, starting
at 90 days of storage, caused by the degradation of antho-
cyanins responsible for the red color. The decrease in the color
parameter a* was also reported by Idham et al. (2012), during
the storage period, for anthocyanins of Hibiscus sabdariffa L.
encapsulated with different carriers.
The concentrated extract was the one that presented the
greatest increase in the parameters a* and b* during the
storage, with an increase in red and decrease in blue color,
respectively. The increase in the blue color may be associated
with a decrease in the anthocyanins responsible for this color,
and the sample starts to have more anthocyanins that have
the red color, increasing the parameter a*. The loss of blue
anthocyanins, more pronounced in this sample, shows that
drying with maltodextrin helped to preserve the characteristic
color in atomized samples, mainly because of the encapsu-
lating effect of the carrier agent, and by the reduction in
moisture content in the extract caused by the drying process.
The high content of water increases the instability of antho-
cyanins because, according to Amr and Al-Tamimi (2007), the
presence of this solvent results in greater conversion of these
molecules to their more unstable pseudobase carbinol. Similar
results were obtained by Idham et al. (2012) who encapsulated
the anthocyanic extract of Hibiscus sabdariffa L. in spray dryer
with different carriers, including maltodextrin. These authors
observed that color characteristics were more preserved in the
encapsulated samples than in the non-encapsulated extract.
4. Conclusions
It is possible to produce powdered, water-soluble pigments
of stable color by spray drying with maltodextrin from the
extract of vinication byproducts of the Bordo grape. Among
the process conditions analyzed during the drying of the
extract of peels and seeds of Bordo grape, drying temperature
mainly inuences moisture content and anthocyanin reten-
tion, besides some color parameters. The concentration of the
carrier agent inuences moisture content, anthocyanin reten-
tion, and hygroscopicity of the samples. Moisture sorption
isotherms, and mainly the color parameter luminosity (L*),
were also inuenced by the concentration of the carrier agent.
The properties of the spray dried samples with maltodextrin,
such as low moisture content, low hygroscopicity, high solubil-
ity, and high color stability, indicate that this byproduct, which
currently has little or no commercial value, may be used as a
natural pigment.
Acknowledgment
The authors would like to thank Coordenaco de
Aperfeicoamento de Pessoal de Nvel Superior (CAPES)
for the scholarship conceded to Volnei Brito de Souza.
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