LWT - Food Science and Technology 94 (2018) 79–86

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LWT - Food Science and Technology

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

Physicochemical properties of tucumã (Astrocaryum aculeatum) powders T

with different carbohydrate biopolymers
Renata S. Silvaa, Carolina de L. Santosa, Josiana M. Marb, Ariane M. Kluczkovskic,
Jayne de A. Figueiredod, Soraia V. Borgesd, Amr M. Bakrye, Edgar A. Sanchesb,
Pedro H. Campeloa,b,∗
a
Faculty of Agrarian Science, Federal University of Amazonas, Manaus, AM, Brazil
b
NANOPOL – Laboratory of Nanostructured Polymers, Federal University of Amazonas, Manaus, AM, Brazil
c
Faculty of Pharmaceutical Science, Federal University of Amazonas, Manaus, AM, Brazil
d
Department of Food Science, Federal University of Lavras, Lavras, MG, Brazil
e
College of Food Science and Technology and MOE Key Laboratory of Environment Correlative Dietology, Huazhong Agricultural University, Wuhan, China

A R T I C LE I N FO A B S T R A C T

Keywords: This work investigated the physico-chemical properties of tucumã pulp (Astrocaryum aculeatum) encapsulated
Astrocaryum aculeatum with different biopolymers. Gum arabic, Maltodextrin, Dextrin (Capsul®) and Modified Starch (SnowFlake®) were
Freeze-drying used as wall material. The pulp/wall material solution was prepared in an 85:15 ratio. The microparticles were
Sorption isotherms obtained from freeze-drying of the tucumã solutions. The pulp composition, physicochemical properties
Vapor adsorption kinetic
(moisture content, water activity, size and morphology) of the microparticles, sorption isotherms, water ad-
Thermogravimetric analysis
sorption kinetics, thermogravimetrics (TGA) and content of different bioactive compounds (antioxidant, phe-
nolic compounds, carotenoids and vitamin A) were all analyzed. The powders presented typical morphology of
products dehydrated by freeze drying, with vacuoles and surface defects of the microparticles. The DX treatment
showed lower hygroscopic behavior, favoring the stability of the tucumã powder. Better bioactive compound
retention values were observed for microparticles with modified starches. GA and MD showed better thermal
resistance compared to modified starches. In general, the biopolymers showed good maintenance of the
bioactive compounds of the encapsulated tucumã.

1. Introduction extend shelf life is through he use of microencapsulation techniques

The Amazon region has one of the largest diversity of native and
exotic fruit species. These include tucumã (Astrocaryum aculeatum), a
fruit with attractive sensory and nutritional characteristics, with the
economically viable potential of its exploitation. The tucumã has a
succulent fruit, with low acid and sugar content, high content of β-
carotene and high energy value. A previous study (Sagrillo et al., 2015)
showed that the pulp of the tucumã is rich in bioactive compounds such
as flavonoids (26.06 mg.100 g-1), b-carotene (20.97 mg.100 g-1) and
rutin (14.51 mg.100 g-1). Tucumã is also used for pharmacological and
cosmetic purposes. The amount of β-carotene, precursor of vitamin A, is
related to the antioxidant potential of the fruit (Da Costa, Leeuwen, &
Costa, 2012; Yuyama, Maeda, Pantoja, Aguiar, & Marinho, 2008).
In the food industry, the shelf life of a product depends on its
quality, which is determined by testing the expiration date, a primary
factor from the consumer's point of view and food safety. One way to
that aim to increase food stability during storage (Jimenez, García, &
Beristain, 2004). Freeze-drying is a dehydration process consisting of
the sublimation of frozen water in vacuum chambers (Liapis & Bruttini,
2015). The freeze-drying technique is the most suitable for heat sensi-
tive foods with several studies proving its efficiency in food stabiliza-
tion (Ezhilarasi, Indrani, Jena, & Anandharamakrishnan, 2013; Fang &
Bhandari, 2012).
Among the encapsulating agents traditionally employed, gum
Arabic is an effective wall material; however, high cost and limited
supply restrict its use. Gum Arabic increase the viscosity of solutions,
forming particles of high size (Tonon, Pedro, Grosso, & Hubinger, 2012)
and can reduce the quality of the fruit extracts encapsulated. A viable
alternative is to use maltodextrins, dextrins and modified starches as
encapsulating agents.
Maltodextrins are carbohydrates formed from the partial hydrolysis
of corn starch, presenting good encapsulation capacity and good

∗
Corresponding author. Faculty of Agrarian Science, Federal University of Amazonas, Manaus, AM, Brazil. Tel.: +55 (92) 99300 1545; fax: +55 (92) 3305 1798.
E-mail address: pedrocampelo@ufam.edu.br (P.H. Campelo).

https://doi.org/10.1016/j.lwt.2018.04.047
Received 21 February 2018; Received in revised form 14 April 2018; Accepted 16 April 2018
Available online 17 April 2018
0023-6438/ © 2018 Published by Elsevier Ltd.
R.S. Silva et al.
protection for lipid oxidation (Gharsallaoui, Roudaut, Chambin,
Voilley, & Saurel, 2007). For encapsulation of fruit extracts, mal-
todextrin is very indicative with good results in the maintenance of
bioactive compounds (M. I. S. Oliveira, Tonon, Nogueira, & Cabral,
2013; Tonon, Brabet, & Hubinger, 2010).
Modified starches (such Capsul® and Snow-Flake®) are carbohy-
drates that present modifications in their chemical structure to improve
their technological properties. Modification techniques improve the
properties of the starches, reducing the tendency of the pastes to form
gels, increasing the pastes stability, reducing the gels viscosity and in-
crease of emulsifying power among others (Damodaran & Parkin,
2017). One of the most recent applications of starch in the food industry
is encapsulating agent (Carneiro, Tonon, Grosso, & Hubinger, 2013;
Zabot, Silva, Azevedo, & Meireles, 2016).
Due to the few studies on microencapsulation of Amazonian fruits,
this work aims at the physical-chemical characterization and stability of
encapsulated microparticles of tucumã using different biopolymers
(gum Arabic, dextrin, modified starch and maltodextrin) as wall ma-
terial. The centesimal composition of the tucumã pulp and the hu-
midity, water activity, particle size, scanning electron microscopy, hy-
groscopicity, sorption isotherm, thermogravimetric analysis and
bioactive compounds content were analyzed.
2. Materials and methods
2.1. Materials
Tucumã fruit (Astrocaryum aculeatum), with high maturation, was
acquired in the local commerce. Four different biopolymers were used
as encapsulating material: Modified Starch SnowFlake® 6704
(Ingredion, Campinas, Brazil) (MS), Gum Arabic (Alland & Roberts,
France) (GA), Maltodextrin DE10 (Ingredion, Campinas, Brazil) (MD)
and Dextrin Capsul® (Ingredion, Campinas, Brazil) (DX).
2.2. Methods
2.2.1. Tucumã juice production
The fruits (∼30 kg) were sanitized with distilled water and hypo-
chlorite solution (2 g.100 g −1 of water; Synth, São Paulo, Brazil) for
10 min. The fruits were then peeled to obtain the extract and homo-
genized in industrial blender with 1:3 (extract/water). The tucumã
extract was filtered using vacuum filtration and the permeate was
conditioned under freezing conditions (−18 °C) until further analysis.
2.2.2. Centesimal composition
The centesimal composition of the tucumã extract was determined
by methodologies recommended by AOAC (2016).
2.2.3. Production of tucumã microparticles
Four different types of biopolymers (MS, GA, MD and DX) were
mixed with tucumã extract in the ratio 85:15 (tucumã extract: wall
material). The solutions were homogenized in a mechanical stirrer
(110-VER-4K3, New Ethics, Brazil) for 10,000 rpm/5 min at 25 °C. The
solutions were rapidly frozen and subjected to freeze-drying (LabConco
2.5L, LabConco, USA). After drying, the microparticles were subjected
to manual milling until the appearance of fine powder (granulometry
less than 100 mesh of the “US Standard”).
2.2.4. Moisture content and activity water
The moisture content of the tucumã powder were gravimetrically
determined in an infrared thermobalance (MOC-120H, Shimadzu,
Japan). The water activity (aw) of the particles at 25 °C was measured
by an AquaLab Water Activity Meter device (Series 3TE, Decagon,
Pullman, USA).
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LWT - Food Science and Technology 94 (2018) 79–86
2.2.5. Solubility and wettability
Solubility was determined using the method proposed by Cano-
Chauca, Stringheta, Ramos, and Cal-Vidal (2005). The tucumã powder
wettability was defined as the time needed for complete dissolution of
1 g of product in 100 mL of distilled water at 25 °C in a 250 mL beaker,
according to the methodology described by (Fuchs et al., 2006) with
some modifications.
2.2.6. Particle size and morphology
The particle size of the tucumã powders was determined at room
temperature using a laser diffraction instrument (Mastersizer 2000,
Malvern Instruments, Worcestershire, UK). The polydispersity index
(span) was calculated according to Equation (1). SEM experiments were
performed using a Supra 35, Carl Zeiss, 1.0 kV. A powder sample was
deposited on a carbon tape and the surface morphology was analyzed at
room temperature.
d 90 − d10
Span =
d50 (1)
d10, d50 and d90, which are the equivalent volume diameters at 10%,
50%, and 90% cumulative volume, respectively.
2.2.7. Sorption isotherms
Sorption isotherms of tucumã powders were determined according
to the static method using saturated salt solutions at 25 °C. The study
involved seven saturated salt solutions with water activity (aw) ranging
from 0.113 to 0.843 and was conducted to constant weight (∼15 days).
The model fit was evaluated on the basis of percentage values of the
average relative deviation, E (%) (Equation. 2):
100
n
Y − YP ⎞
E (%) =
n
∑⎛ Y
i=1 ⎝ ⎠ (2)
where n is the number of observed data, Y is the moisture content
observed value, and YP is the moisture content model predicted value.
2.2.8. Water adsorption kinetic
Approximately 0.5 g of powdered tucumã were packed in containers
with saturated NaCl solution with controlled relative humidity
(RH = 75%) to constant weight at 25 °C. The amount of adsorbed water
(hygroscopicity) was calculated as a percentage relative to the dry base
of the microparticles (Campelo-Felix et al., 2017). In order to know the
water diffusion mechanism in the microparticles, the hygroscopicity
data were adjusted to the interparticular diffusion model (Equation
(3)):
1
qt = C + kid t 2 (3)
where C is the intercept, kid is the intraparticle diffusion rate constant
(mg/g.h1/2) and t is the contact time.
2.2.9. Thermogravimetric analysis
The thermal stabilities of tucumã microparticles were evaluated
through thermogravimetric analysis (TGA) on a TG-DTA H Shimadzu
60 (Shimadzu Corp., Kyoto, Japan) under nitrogen atmosphere
(10 mL min−1) with heating from 25 to 550 °C at a rate of 10 °C.min−1.
2.2.10. Bioactive compounds
Antioxidant activity DPPH (Tonon et al., 2010) and ABTS (L. B. da
Silva et al., 2016); phenolics compounds (Borges et al., 2016); β-car-
otene and vitamin A (Yuyama et al., 2008) juices and microparticles
were analyzed to predict the influence of the type of wall material on
the maintenance of the tucumã functional properties according to
specific methods.
2.2.11. Statistical analysis
R software was used for analysis of variance (ANOVA) as a way of
R.S. Silva et al. LWT - Food Science and Technology 94 (2018) 79–86

Table 1 that hinder the diffusion of water during drying, retaining a higher
Centesimal composition of tucumã pulp. moisture content in microparticles (Ezhilarasi, Indrani, Jena, &
Parameters Concentration (g.100g−1 of pulp) Anandharamakrishnan, 2014).
Wettability is the time required for reconstitution of powders in
Moisture content 46.25 ± 0.23 water (Fernandes, Borges, Botrel, & Oliveira, 2014b) and is related to
Ash 1.2 ± 0.42
the content and physicochemical characteristics of encapsulated mate-
Fat 35.42 ± 0.66
Proteins 3.65 ± 0.21
rials such as material type, shape and particle size and reconstitution
Carbohydrates 13.99 ± 0.45 temperature in water (Botrel et al., 2017b; Vissotto, Montenegro,
Santos, & Oliveira, 2006). The wettability of tucumã powders with
different biopolymers presented a significant difference (p < 0.05),
evaluating the effects of different carrier agents on the properties of the with lower values for GA and MD samples, respectively. Blackberry
tucumã extract powders obtained by freeze-drying. Differences between powder (Ferrari, Germer, Alvim, Vissotto, & de Aguirre, 2012) also
the mean values obtained for each property were evaluated at a 5% showed higher wettability for GA compared to MD. It is important to
significance level (p ≤ 0.05) using the Tukey's test. All methods were find biopolymers that have low wettability times to prevent non-hy-
performed in triplicates, except for the thermal analysis. drated microparticles during reconstitution (Oliveira et al., 2018).
Solubility is a factor used to characterize the stability of micro-
3. Results particles after dissolution. At first, this variable is related to matrix
material (Yousefi, Emam-Djomeh, & Mousavi, 2011). Powdered foods
3.1. Centesimal composition must have high solubility, it being a decisive factor in the quality of
these products (Fernandes, Borges, & Botrel, 2014a). As expected, all
Table 1 shows the centesimal composition of tucumã extract. The samples showed high solubility (85.12–91.44 g microparticles.100 g−1
tucumã is characterized as a non-succulent fruit, with low sugar content of water), a common feature of biopolymers formed from carbohydrates
and acid content. The fruit is composed mostly of lipids, carbohydrates (Oliveira et al., 2013) and fruit extracts had few water insoluble com-
and proteins. The moisture, ash, carbohydrate, protein and lipid con- ponents. Other authors also observed high solubility for microparticles
tents also corroborated with those of other studies (Ferreira, Lucien, of strawberry extract (Oliveira et al., 2013) and pomegranate juice
Amaral, & Silveira, 2008; Yuyama et al., 2008). (Jafari, Ghalegi Ghalenoei, Dehnad, Ghalenoei, & Dehnad, 2017).

3.2. Physicochemical properties 3.3. Particle size

The physico-chemical properties of freeze-dryed tucumã are pre-
sented in Table 2. Water activity (Aw) is an important parameter to
predict the microbiological quality of food. Fungi grow at Aw > 0.62
and bacteria Aw > 0.86. No treatment presented water activity values
that favored microbial growth. The different wall materials presented
significant difference (p < 0.05) for water activity values. MD pre-
sented lower Aw when compared to other treatments. This can be ex-
plained by the low hygroscopicity of MDs, reducing the amount of free
water on the surfaces (Campelo et al., 2017). Other authors also ob-
served lower water activity values for treatments with MD compared to
other biopolymers in the encapsulation of Rubus fruticosus (Díaz,
Beristain, Azuara, Luna, & Jimenez, 2015) and açaí juice (Tonon,
Brabet, Pallet, Brat, & Hubinger, 2009b).
Tucumã microparticles presented high moisture content value
(Table 2) with values of 7.54–8.03 g water/100 g dry power. The type
of wall material varied significantly, with the highest values observed
for GA, MD and DX. The differences observed are related to different
properties of the encapsulation matrices because the interaction of
water with each biopolymer depends on the molecular properties and
capacities of its binding to water, becoming unavailable for chemical,
biochemical, physicochemical or microbiological deterioration reac-
tions (Silva, Zabot, Cazarin, Maróstica, & Meireles, 2016c). Powdered
foods obtained by freeze drying have a porous structure due to the
sublimation of the ice crystals. When the freezing temperature is very
low (below −40 °C) the ice crystals are smaller, forming small pores
Particle size is an important characterization in the analysis of
powder quality, since the presence of larger particles can reduce the
exposure of the powder to oxygen, protecting against oxidation, that is,
the smaller the particle size, the higher the surface deterioration of
compounds susceptible to deterioration. Powdered tucumã showed
particle size (Table 2) with high values, varying in the range from 89.45
to 105.71 μm. This can be explained by the fact that the particles are
not atomized during drying, forming rigid structures with the need for
maceration or dry mass grinding (C. Chen, Chi, & Xu, 2012; Silva et al.,
2016c). Other authors also observed large-size particles by freeze-
drying of annatto oil (Silva, Zabot, & Meireles, 2015). When relating
different biopolymers, other authors (Tonon et al., 2012) also observed
larger particles for linseed oil microencapsulated with GA compared to
MS. The branched structure with long chains of gum Arabic is re-
sponsible for its higher viscosity (Tonon et al., 2012).
The polydispersity index (PDI) is related to the homogeneity of the
particle size distribution, an important factor for studies of controlled
release, texture and dispersibility of microencapsulated substances
(Silva, Azevedo, Cunha, Hubinger, & Meireles, 2016a). The PDI values
presented a significant difference (p < 0.05), with more homogeneous
GA particles in relation to the other biopolymers. These values are
confirmed by the particle size distribution profile (Fig. 1), with a nar-
rower distribution peak for the tucumã powder with GA. Flaxseed oil
particles with GA were less homogeneous compared to samples with MS
(Tonon et al., 2012).

Table 2
Activity water, moisture content, particle size and span of tucumã powders.
Assay Activity water (aw) Moisture content (g water.100g−1 dry powder) Wettability Solubility Particle size (μm) Span
(s) (g microparticles.100g−1 of water)

GA 0.41 ± 0.02a 8.03 ± 0.5a 194 ± 3.45 b 85.12 ± 2.45 a

105.71 ± 5.63a 1.65 ± 0.23c
MD 0.36 ± 0.02b 7.89 ± 0.4 a 170 ± 1.23 c 91.44 ± 1.45 a
94.33 ± 4.56b 2.51 ± 0.65b
MS 0.43 ± 0.01a 7.54 ± 0.5 b 223 ± 4.22 a 85.23 ± 1.23 a
89.45 ± 3.33b 3.23 ± 0.32a
DX 0.40 ± 0.01a 7.88 ± 0.2 a 212 ± 3.06 a 88.25 ± 2.11 a
92.53 ± 6.22b 2.32 ± 0.12b

a,b,c
Same letter represents no significant difference (p > 0.05). Results are presented as the mean ± standard deviation. GA: Gum Arabic; DX: dextrin; MD:
maltodextrin; MS: Modified Starch.

81
R.S. Silva et al.
Fig. 1. Particle size distribution for tucumã powders. GA: GA; DX: dextrin; MD:
maltodextrin; MS: Modified Starch.
3.4. Scanning electron microscopy (SEM)
Fig. 2 presents the SEM images for the tucumã microparticles. Mi-
crographs are important tools to analyze the formation of micro-
particles using different wall materials and drying processes (Silva,
Zabot, Bargas, & Meireles, 2016b). Note that the surfaces are irregular,
with sharp edges and considerable indentations resulting from the
powder maceration process. There are also regions with vacuoles re-
lated to the space occupied by the ice crystal before drying (Ezhilarasi
et al., 2013). This behavior is typical of microparticles produced by
freeze-drying, as observed by other authors (Caparino et al., 2012).
Microparticles with MS tended to form spherical structures. This may
be related to the good surface activity of the biopolymer, producing
more uniform structures.
3.5. Sorption isotherms
The quality of powdered foods depends on the moisture content, the
moisture migrated or adsorbed during storage (Fernandes et al., 2013).
Table 3 shows the coefficients of the sorption isotherm models adjusted
for the experimental data of tucumã powder. The GAB, Smith, Hen-
derson and Halsey models were used to describe the hygroscopic be-
havior of the microparticles. Mathematical models with values of E
(%) < 10 are considered equations of good fit (Lomauro, Bakshi, &
Fig. 2. SEM images of tucumã powder with different biopolymers.
82
LWT - Food Science and Technology 94 (2018) 79–86
Labuza, 1985). Fig. 3 shows the experimental values and the predicted
sorption isotherms curves for the GAB model. All curves are Type III,
characteristic of products rich in starch (Toledo Hijo et al., 2015). A
Type III curve was also observed for fish oil microparticles with GA
(Botrel et al., 2017a), lemon juice with MD and GA (Martinelli, Gabas,
& Telis-Romero, 2007) and strawberry pulp with DX, GA and MD (M. I.
S. Oliveira et al., 2013). All treatments presented low water adsorption
values until a water activity lower than 0.6. After these values, a large
increase of the water adsorption by the microparticles is observed.
Mainly due to their molecular structure and high hygroscopicity, the
microparticles with GA had a higher moisture content than the other
treatments. Under low relative humidity, the water can be adsorbed on
the surface of carbohydrates in the polar active sites, while at high
water activity values, the carbohydrate dissolution occurs (Fernandes,
Borges, & Botrel, 2014a).
Fig. 4 shows the appearance of the microparticles after packaging at
different relative humidity values. Note that the DX did not present
structural change, that is, it did not present phase change from the
vitreous state to the gummy state. Powdered foods tend to agglomerate
due to surface wetting (Mathlouthi & Rogé, 2003). The other materials
presented phase change at 54% (MD), 76% (GA) and 86% (MS). In
microencapsulation studies of Swiss cheese bioaroma with a mixture of
MD and DX Capsul® (Costa et al., 2015), the authors observed a tran-
sition from vitreous to gummy in water activities above 67% at 25 °C.
Water can cause a plasticizer effect in amorphous systems, increasing
polymer chain mobility (Costa et al., 2015), allowing oxygen, light and
moisture to enter the microparticles, reducing the stability of en-
capsulated bioactive compounds. Other authors (Tonon et al., 2009a)
observed phase transition for GA and MD in water activity close to 0.6
for açaí microparticles, corroborating values in this present work. In-
creasing the moisture content after water adsorption may cause various
changes in the encapsulation matrix causing particle agglomeration or
reduction of the glass transition temperature compromising the
polymer matrix efficiency (Silva et al., 2016b).
3.6. Water sorption kinetic
The coefficients adjusted for water adsorption kinetics models are
presented in Table 4. All models presented a good fit, with E (%) values
lower than 10. The pseudo first order model was considered the best fit
since it presented the lowest mean values of E (%). The coefficient qe,
related to the equilibrium moisture of the powders at equilibrium,
confirms the higher hygroscopicity for treatments with GA in relation to
the other biopolymers.
R.S. Silva et al. LWT - Food Science and Technology 94 (2018) 79–86

Table 3
Models parameter to tucumã powder sorption isotherms at 25 °C.
Models Coefficients GA MD MS DX

−1
GAB X0 (g of water.100g water) 5.599 4.752 5.329 4.275
X eq =
X 0 . C . K . Aw C 1.363 4.235 3.947 4.068
(1 − K . Aw) . (1 − K . Aw + C . K . Aw) K 0.954 0.951 0.899 0.806
E (%) 9.652 11.235 7.698 12.456
Halsey A 3.749 6.213 8.656 7.977
1 B 0.962 1.189 1.311 1.534
X eq = ( A
)
ln (Aw)
B
E (%) 12.652 15.478 13.465 16.446
Henderson A 0.196 0.123 0.085 0.092
log (1 − Aw) B
−1 B 0.707 0.899 1.033 1.218
X eq = ( −a ) E (%) 9.541 16.546 11.236 32.456
Smith A −2.561 −0.312 0.256 0.984
X eq = A + B. log (1 − Aw) B 13.78 10.87 10.488 5.985
E (%) 14.568 17.566 18.236 12.225

Xeq, moisture content; Aw, water activity; X0, monolayer moisture content; A, B, C and K, models coefficients; and E(%), relative mean error. GA: Gum Arabic; DX:
dextrin; MD: maltodextrin; MS: Modified Starch.

The dTGA curves confirm these stages. It is noted that all biopolymers
present degradation at 200–330 °C, with greater initial loss for DX mi-
croparticles. MD and GA showed higher degradation temperature, re-
maining stable up to 280 °C. In studies of phenolic coffee compounds
(Ballesteros, Ramirez, Orrego, Teixeira, & Mussatto, 2017), the authors
observed that the microparticles with GA presented thermal stability
similar to MD. (Zabot et al., 2016) observed that the use of modified
starches improved the thermal stability of oregano extract micro-
particles when compared to inulin. The biopolymers used present a
mass loss of 56% for GA (Zohuriaan & Shokrolahi, 2004), 64% for MD
(Ballesteros et al., 2017), 65% for MS Snow-Flake® (Silva et al., 2016a)
and 60% for DX Capsul® (Costa et al., 2015) in the second stage. The
lower the mass loss, the more stable the biopolymer in thermal pro-
cesses (Costa et al., 2015). Therefore, the thermal resistance of the
biopolymer may be related to the enhanced protection of the en-
capsulated bioactive compound.

3.8. Bioactive compounds

Fig. 3. Sorption isotherms for tucumã powder at 25 °C. GA: GA; DX: dextrin;
MD: maltodextrin; MS: Modified Starch.
Fig. 5 shows the experimental and adjusted data for the pseudo first
order model for the tucumã powder. All treatments presented rapid
water adsorption before the first 20 h, with reduction of adsorption
velocity and reaching equilibrium before 40 h. The initial moisture
absorption was due to the filling of capillaries on the microparticles
surface, while in the adsorption velocity reducing step due to the free
space for water binding (Kim & Rhim, 2004). GA has a large number of
branches with hydrophilic groups favoring water adsorption, while
MDs have a higher molecular weight with less hydrophilic groups (M. I.
S. Oliveira et al., 2013). For better preservation and stability of pow-
dered foods, lower water absorption values are desirable, improving
reconstitution properties and reducing particle agglomeration
(Fernandes, Borges, & Botrel, 2014a).
It can be observed that the curves present similar behavior, with
rapid water adsorption in the first hour, with reduction of the rate until
equilibrium. After 3 h of storage, the curves showed small water ad-
sorption peaks, momentarily increasing the amount of solvent ad-
sorbed. This can be explained by the relaxation of the polymer chains
due to the high humidity, exposing active sites to new connections with
water (Pérez-Alonso, Beristain, Lobato-Calleros, Rodríguez-Huezo, &
Vernon-Carter, 2006).
3.7. Thermogravimetric analysis
The TGA curves for the tucumã microparticles are shown in Fig. 6.
The main purpose of the microencapsulation processes is to main-
tain the physical and chemical characteristics of bioactive compounds
during storage, protecting them from oxidative and degradation pro-
cesses (Silva et al., 2016c). The bioactive compound level values (an-
tioxidants, phenolics, β-carotene and vitamin A) are shown in Table 5.
For all the parameters a significant difference (p < 0.05) was observed
for all treatments, with higher retention of the bioactive compounds for
samples encapsulated with DX and MS. Only for phenolic compounds
did the GA microparticles present better results. Similar values of β-
carotene (10,286.38 μg.100mL−1) and vitamin A (857.20 μg.100mL−1)
were observed for tucumã juice in other studies (Yuyama et al., 2008).
In microencapsulation studies of açaí juice (Tonon et al., 2010) better
protection of bioactive compounds was also observed when using MD
compared to GA. Lower DPPH values were also observed for micro-
encapsulated extracts from freeze-dried grapes with GA, polydextrose
and guar gum compared to the natural extract (Kuck & Noreña, 2016).
This can be explained by the moisture content (Table 2) and hygro-
scopic characteristics of the wall materials (Fig. 5), since the more
water in the microparticles, the greater the possibility of bioactive
compound degradation.
Although the lyophilization process presents little damage to the
chemical characteristics of fruit juices due to the use of low tempera-
tures in the drying process (Agudelo, Barros, Santos-Buelga, Martínez-
Navarrete, & Ferreira, 2017), the different types of wall materials in-
fluenced the retention of these compounds. This reduction of freeze-
dried bioactive compounds has also been observed in studies of cassava
pulp (Eugenia uniflora) and jambolon (Syzygium cumini) (Borges et al.,
2016).

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R.S. Silva et al. LWT - Food Science and Technology 94 (2018) 79–86

Fig. 4. Physical aspects of the tucumã powder produced using the different wall materials in the water activity range of 0.11–0.84. GA: GA; DX: dextrin; MD:
maltodextrin; MS: Modified Starch.

Table 4
Model coefficients for water vapor adsorption in tucumã powders at 25 °C and
relative humidity to 75%.
Assay Pseudo First-order Pseudo second-order
q = qe (1 − e−kt ) k 2 qe2 t
q=
1 + k 2 qe2 t

k (h−1) qe E (%) k2 [mg.(g.h)−1] qe E (%)

GA 0.11 21.95 2.89 5.14 24.43 4.59

MD 0.13 19.52 5.78 0.24 226.47 6.23
MS 0.17 16.60 3.65 0.56 139.09 2.90
DX 0.29 11.67 4.33 0.85 347.99 7.55

qe, amount of water adsorbed at equilibrium; k, model's constant; and E(%),

relative mean error. GA: Gum Arabic; DX: dextrin; MD: maltodextrin; MS:
Modified Starch.

Fig. 6. Thermogravimetric curves for tucumã powder with different biopoly-

mers: TGA (A) and dTGA (B).

4. Conclusion

Fig. 5. Hygroscopicity profile for tucumã powders at 25 °C. GA: GA; DX: dex- The freeze-drying technique and the different biopolymers were
trin; MD: maltodextrin; MS: Modified Starch. efficient for the reconstitution properties of the powdered tucumã,
presenting high solubility and good reconstitution time (wettability).

84
R.S. Silva et al.
Table 5
Antioxidant content, Total Phenolics, β-carotene and Vitamin A to tucumã juice and encapsulated.
Parameter Tucumã juice GA
a c
DPPH (EC50) 40.5 ± 1.23 29.5 ± 0.2
ABTS (μmolTE/mL) 1424 ± 102 a 1323 ± 99 b
Phenolics (mg galic acid/100 g) 654.7 ± 2.3 a 632.2 ± 11.2 a
β-carotene (μg/mL) 67.45 ± 1.24 a 54.22 ± 2.45 b
Vitamin A (μg/mL) 0.14 ± 0.01 a 0.09 ± 0.01 b
a,b,c
Same letter represents no significant difference (p > 0.05). Results are presented as the mean ± standard deviation. GA: Gum Arabic; DX: dextrin; MD:
maltodextrin; MS: Modified Starch.
The powders presented typical morphology of products dehydrated by
freeze drying, with vacuoles and surface defects of the microparticles.
The DX treatment showed lower hygroscopic behavior, favoring the
stability of the tucumã powder. Better bioactive compound retention
values were observed for microparticles with modified starches. It is
suggested the stability of these powdered foods under different storage
conditions and the application in food matrices be studied.
Acknowledgements
The authors are grateful to Innova (Manaus, Amazonas, Brazil) for
support with particle size analysis and the Faculty of Technology,
Federal University of Amazonas, for assistance in thermogravimetric
analysis.
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