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Bioactive films based on babassu mesocarp flour and starch

Article  in  Food Hydrocolloids · April 2017

DOI: 10.1016/j.foodhyd.2017.04.022


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4 authors:

Bianca C. Maniglia Larissa Tessaro

University of São Paulo University of São Paulo


Alessandra Lucas D.R. Tapia-Blácido

Universidade Federal de São Carlos University of São Paulo


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Food Hydrocolloids 70 (2017) 383e391

Contents lists available at ScienceDirect

Food Hydrocolloids
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Bioactive films based on babassu mesocarp flour and starch

cido a, *
Bianca C. Maniglia a, Larissa Tessaro a, Alessandra A. Lucas b, Delia R. Tapia-Bla
Departamento de Química, Faculdade de Filosofia, Ci^ ~o Preto, Universidade de Sa
encias e Letras de Ribeira ~o Paulo, Ribeira
~o Preto, SP, CEP: 14040-90, Brazil
Departamento de Engenharia de Materiais, Universidade Federal de Sa ~o Carlos, Sa
~o Carlos, Sa
~o Paulo, CEP: 13565-905, Brazil

a r t i c l e i n f o a b s t r a c t

Article history: This work aimed to evaluate the properties of films prepared with babassu mesocarp flour or with starch
Received 20 March 2017 isolated from babassu mesocarp by steeping in water (WS), alkaline steeping (KS), or acid steeping (AS).
Received in revised form The films were obtained by casting; glycerol was used as plasticizer. Although the babassu flour pre-
18 April 2017
sented high content of amylose, its major content of protein and fiber afforded a less mechanically
Accepted 18 April 2017
Available online 19 April 2017
resistant, more flexible, more opaque, more hydrophilic, more water vapor-permeable film with greater
capacity to absorb water as compared to the babassu starch films. The WS, AS, and KS methods yielded
purer starches with different contents of amylose, lipids, fibers, and total phenolic compounds, which
Agroindustrial residues
influenced the mechanical and functional properties of the starch films. Due to its major content of
Babassu mesocarp amylose, the WS starch film was stronger, more rigid, less soluble, less water vapor-permeable, and more
Starch crystalline than the AS and the KS starch films. X-ray diffraction and SEM reveled that the WS starch film
Flour had denser and more ordered and homogeneous structure. However, the AS starch film had the highest
Bioactive film antioxidant activity (70%) due to the largest amount of total phenolic compounds. The babassu flour and
starch films exhibited good antioxidant activity, so they can be used as materials for packaging of
oxidation-sensitive foods.
© 2017 Elsevier Ltd. All rights reserved.

1. Introduction Babassu mesocarp, a byproduct of the babassu oil extraction

industry, is produced during the separation of the babassu coconut
Biodegradable films have emerged as an environmentally almonds. In 2014, 89.79 tons of babassu coconuts were harvested in
friendly strategy to decrease the pollution originating from the the Northeastern, Northern, and Central Western regions of Brazil
accumulation of synthetic plastic waste. However, the application (IBGE, 2015; Machado, Chaves, & Antoniassi, 2006; Soler, Vitali, &
of these materials will only be feasible if they are competitive in Muto, 2007). The babassu oil corresponds to only 7% of the total
terms of cost and functionality as compared to synthetic plastics. weight of the fruit; the other parts like the epicarp, the endocarp,
This might be possible if cheaper raw materials such as agro- and the mesocarp (93%) are underused as biomass (Teixeira, 2008).
industrial byproducts are used. This type of raw material may The babassu endocarp and epicarp have high content of fixed car-
contain biopolymers such as protein, fiber, and starch, so it can be bon, which makes them more suitable for carbonization and
employed to produce films. These byproducts may also contain burning than the babassu nuts and mesocarp, which contain less
bioactive compounds like antioxidants and antimicrobials, which than 5% fixed carbon (Teixeira, 2008). The babassu mesocarp is
allows the production of bioactive films that offer extra benefits in usually transformed into flour and used as animal feed. In a pre-
relation to conventional materials (Andrade-Mahecha, Tapia- vious work, Maniglia and Tapia-Bl acido (2016) demonstrated that
Blacido, & Menegalli, 2012; Chandra & Rustgi, 1998; Daudt et al., the babassu mesocarp flour displays antioxidant activity due to the
2016; Dias, Müller, Larotonda, & Laurindo, 2010; Maniglia, presence of phenolic compounds. These authors isolated starch
Domingos, de Paula, & Tapia-Bla cido, 2014; Pelissari, Andrade- from the babassu mesocarp flour by two methodologies, steeping
Mahecha, Sobral, & Menegalli, 2013; Salas-Valero, Tapia-Bl acido, in water and steeping in alkaline pH. These methodologies pro-
& Menegalli, 2015). vided starch with distinct chemical composition and functional
characteristics. However, the isolation of starch did not remove the
phenolic compounds, so the final starch still had antioxidant ac-
tivity, which made it an interesting material to obtain bioactive
* Corresponding author.
films. Antioxidant activity is a desirable feature in materials that are
E-mail address: (D.R. Tapia-Bla
0268-005X/© 2017 Elsevier Ltd. All rights reserved.
384 B.C. Maniglia et al. / Food Hydrocolloids 70 (2017) 383e391

used to cover fruits, meats, and cheeses, which are all sensitive to by an enzymatic method (amylase, protease, amylo-glucosydase
oxidation. Bioactive starch films have been produced through the enzymes) by means of the AOAC 985.29 methodology (AOAC,
addition of antimicrobial and antioxidant agents such as tannic acid 1990). The content of starch was calculated by difference. The
(Pyla, Kim, Silva, & Jung, 2010), cinnamon and propolis essences content of amylose was analyzed by the simplified iodine colori-
(Kechichian, Ditchfield, Veiga-Santos, & Tadini, 2010), potassium metric method, according to the methodology proposed by Juliano
sorbate and chitosan (Shen, Wu, Chen, & Zhao, 2010), ferulic acid (1971) and adapted by Martínez and Cuevas (1989).
(Mathew & Abraham, 2008), mango pulp and mate (Reis et al.,
2015), and butter milk (Moreno et al., 2014) to the film. Research 2.4. Preparation of babassu films
into films produced from agroindustrial residues bearing antimi-
crobial and antioxidant natural agents is scarce in the literature. In a The films were prepared by casting from a suspension of 4%
previous work, Maniglia et al. (2014, 2015) prepared films from the starch or babassu mesocarp flour (w/w) in deionized water. This
extraction residue of turmeric pigment, to find that the film suspension was homogenized with a magnetic stirrer (IKA® C
exhibited antioxidant activity due to the presence of curcuminoids. eMAG HS7, Marconi, Piracicaba e Brazil) for 30 min. Then, the
This work aims: (1) to compare the mechanical and functional suspension was heated at 81  C for 30 min, the plasticizer glycerol
properties of babassu mesocarp flour and starch films (designated was added (19 g of plasticizer/100 g of starch), and the suspension
flour film and starch film, respectively), and (2) to evaluate how the was finally heated for 15 min. Subsequently, the solution was
methodology used to isolate babassu starch (steeping in acid, in poured onto acrylic plates, a weight of 0.15 g/m2 was maintained,
water, or in alkaline medium) affected the properties of the starch and the plates were dried at 35  C (45% RH) for 10 h in an oven with
films. forced circulation (SL 200e364, SOLAB®, PiracicabaeBrazil). Before
characterization, all the films were preconditioned for at least 48 h
2. Material and methods in desiccators containing saturated solution of sodium bromide
(58% RH).
2.1. Material
2.5. Optical properties of the films
The babassu mesocarp flour was provided by industry “Coo-
paesp” (Esperantinopolis e Maranha ~o, Brazil). The flour was sieved
The color and opacity of the films were determined on a
(80 meshe0.180 mm) and stored at 10  C. portable colorimeter MiniScan XE (Hunterlab e Riston, Virgínia,
Sodium Hydroxide and Ascorbic Acid P.A. were acquired from EUA) according to the Hunterlab method (1997). A CIE-Lab color
Dynamic e Contemporary Chemistry (S~ ao Paulo, Brazil). The radical scale was used to measure the degree of lightness (L*), redness
DPPH (2,2-diphenyl-1-picrylhydrazyl) was purchased from Aldrich (þa*) or greenness (a*), and yellowness (þb*) or blueness (b*) of
~o Paulo, Brazil). Glycerol P.A. grade was supplied by Sigma-
(Sa the films. The results were expressed as the average of five mea-
Aldrich (S~
ao Paulo, Brazil). surements at different parts of the surface of the film. The total
color difference was calculated on the basis of Equation (2):
2.2. Isolation of babassu starch
Babassu starches were isolated by three different methods: DE* ¼ 2
ðDL* Þ þ ðDa* Þ þ ðDb* Þ ;
2 2
steeping in water (WS), alkaline steeping (KS), and acid steeping
(AS). All the methods involved steeping and wet milling steps. To where DL*, Da*, and Db* are the differences between the L*, a*, and
this end, the babassu mesocarp flour was soaked in deionized water b* parameters of the samples and the standard sample (L* ¼ 93.49,
(neutral pH e 7.0), in a solution of sodium hydroxide 0.25% (alkaline a* ¼ 0.77, and b* ¼ 1.40).
pH e 10.0), or in a solution of ascorbic 1% acid (acid pH e 4.0),
respectively, at a 1:2 ratio, and left to stand at 10  C for 18 h. Then, 2.6. Antioxidant activity and total phenolic compounds
the moist babassu flour was wet milled for 2 min in a food pro-
cessor (Walita) operating at maximum power. The milled material The antioxidant activity of the babassu mesocarp flour, the
was screened through 80-, 200-, and 270-mesh stainless steel babassu mesocarp starches, the flour film, and the starch films was
sieves. The material retained in the sieves was reprocessed and measured by the DPPH methodology (Martins, Cerqueira & Vicente,
sieved again four additional times. The resulting liquid was 2012) as described by Maniglia and Tapia-Bl acido (2016).
centrifuged at 1500  g at 10 ± 2  C for 10 min (Quimis, Q222RM, The content of total phenolic compounds in the babassu
Brasil). The supernatant was discarded, and the starch was re- mesocarp flour, the babassu mesocarp starches, the flour film, and
suspended in water. This process was repeated until the starch the starch films was determined by the Folin-Ciocalteau colori-
reached pH 7.0, for all the methods (WS, KS, and AS). The starch was metric method (Hillis & Swain, 1959). Briefly, 0.5 mL of the diluted
dried in air-circulating oven at 40  C for 6 h (Quimis, Q314M292, sample extract was transferred to tubes containing 0.5 mL of a 1:7
Brazil) and later milled and sieved through 80-mesh sieves. The dilution of Folin-Ciocalteu's reagent in water. After 3 min, 1.0 mL of
final starches were stored in sealed dark flasks at 10  C. a solution of sodium carbonate (0.5 M) was added to the sample.
The tubes were allowed to stand at room temperature for 10 min;
2.3. Chemical composition then, the absorbance at 725 nm was measured on an HP spectro-
photometer (Hewlett Packard 8453, EUA). The content of total
The chemical composition of the babassu mesocarp flour and of phenolic compounds was expressed as mg of gallic acid equivalents
the starches isolated by WS, KS, or AS was determined in triplicate. (GAE)/100 g of sample. All the analyses were performed in
The contents of moisture and ash were analyzed by the AOAC triplicate.
920.151 and 92.303 methodologies, respectively (AOAC, 1997). The
content of proteins was measured by the AOAC 926.86 methodol- 2.7. Mechanical properties of the films
ogy (AOAC, 2005); a nitrogen conversion factor of 6.25 was applied.
The content of lipids was obtained according to the methodology of The mechanical tests were conducted on a texture analyzer TA
Bligh and Dyer (1959). The content of dietary fiber was determined TX Plus (TA Instrument, England). The tensile strength (TS) and the
B.C. Maniglia et al. / Food Hydrocolloids 70 (2017) 383e391 385

elongation at break (E) were obtained according to the ASTM 2.12. Scanning electron microscopy (SEM)
Standard method D882-02 (ASTM, 2002) taking an average of five
determinations in each case. Sample films were cut into 2.54-cm- The morphological characteristics of the babassu films were
wide strips with a length of at least 10 cm. The initial grip sepa- examined by scanning electron microscopy (SEM). The samples
ration and the crosshead speed were set at 80 mm and 1.0 mm/s, were placed on an aluminum specimen stub and covered with gold
respectively. Young's modulus (YM) was calculated as the inclina- with the aid of a cathodic sputter (Sputter Coater, SCD050, USA).
tion of the initial linear portion of the stress versus strain curve by The samples were analyzed under a scanning electron microscope
using the software Texture Expert V.1.22 (SMS). ZEISS model EVO-50 at 20 KV.

2.8. Solubility in water and moisture of the films 2.13. X-ray diffraction (XRD)

The solubility in water of the films was calculated as the per- The samples were placed on an aluminum specimen stub and
centage of dry matter of the solubilized film (discs with diameter of analyzed at ambient temperature (~25  C) on an X-ray diffrac-
20 mm) after immersion in 50 mL of water at 25 ± 2  C for 24 h, tometer Siemens model D5005 (Baden-Württemberg, Germany)
under mechanical stirring, as described by Tapia-Bla cido, Sobral & operating with monochromatic filter, Cu Ka radiation, current of
Menegalli (2011). The content of moisture in the films was deter- 30 mA, and voltage of 40 kV. The scanning rate was 0.02 /s with 2q
mined according to the ASTM Standard method D644-99 (ASTM, angles varying between 2 and 50 . The crystallinity index of the
1999). Small specimens of the films were dried in an oven at materials was quantitatively estimated as the ratio between the
105  C until constant weight was achieved (~24 h). Moisture was crystalline area and the total area of the diffractogram, as described
calculated as the percentage of weight loss relative to the original by Nara and Komiya (1983). The software Origin 6.0 was employed
weight. The analyses were accomplished in triplicate. for this purpose (OriginLab Corporation, Massachusetts, USA).

2.9. Water vapor permeability of the films 2.14. Statistical analysis

The water vapor permeability (WVP) test was carried out by The data were analyzed by analysis of variance (ANOVA) at a 5%
using a modified E96-95 ASTM Standard method (ASTM, 1995) at significance level and by Tukey's test of multiple comparisons with
25 ± 2  C. The film samples were sealed over the circular opening of 95% confidence interval; the Statistica 13.0 software was used.
a permeation cell containing silica gel, and the cells were placed in
desiccators containing distilled water (steady-state condition). The 3. Results and discussion
cell was weighed on an analytical scale every 1 h, for 9 h. The WVP
was calculated as WVP ¼ w.x/t.A.DP, where “x” was the average 3.1. Chemical composition of babassu flour and starches
thickness of the films, “A” was the permeation area of the films
(0.00196 m2), “DP” was the difference between the partial pressure The babassu mesocarp flour furnished by “Coopaesp” presented
of the atmosphere over silica gel and over pure water (3.168 kPa, at higher content of starch (84.57 g/100 g) and lower contents of ash,
25  C); the term w/t was determined by linear regression based on lipid, and protein (1.04 g/100 g, 1.51 g/100 g, 1.77 g/100 g, respec-
weight gain data as a function of time. tively) as well as significant content of dietary fiber (11.11 g/100 g).
Other authors have reported lower content of starch (50e60%) and
2.10. Contact angle measurements higher content of dietary fiber (15e37%) for babassu mesocarp flour
(Baruque Filho, Maria Da Graca & Sant'anna, 2000; Cinelli, Lo pez,
The contact angle was obtained by employing OCA-20 Data- Castilho, Freire, & Castro, 2014). This difference may be due to the
physiscs (OCA 20, Dataphysiscs, Germany). Images of a water drop industrial process the babassu fruit was submitted to, to the par-
(surface tension ¼ 72.7 mN/m) were taken every 2 min in air, at ticularities of the babassu species, and/or to the distinct climatic
room temperature. The image processing software GIMP 2.6.8 was conditions in which the plants were cultivated.
used to measure the contact angle, which was identified as tangent Table 1 reveals that the KS method yielded a purer starch (97 g/
to the edge of the drop, in the intersection of the liquid, solid, and 100 g) because it removed more lipids, fibers, and proteins as
gaseous media. The values of contact angle were determined in compared to the WS and AS methods. Indeed, steeping in alkaline
triplicate. pH solubilized proteins and lipids to a larger extent and cleaved
lignin by saponification of the ester groups and fragmentation of
2.11. Water uptake test hemicellulose polymers, to afford a purer starch and higher process
yield than the WS and AS methods (Ga sp lma
ar, Ka n, & Re czey,
The water uptake tests were performed according to Dufresne, 2007; Li et al., 2012; Machado et al., 2000; Mandal &
Dupeyre, and Vignon (2000). Dried film samples Chakrabarty, 2011; Tukomane, Leerapongnun, Shobsngob, &
(20 mm  20 mm) were conditioned at 25  C in a desiccator con- Varavinit, 2007). Alkaline hydrolysis of lipids can also occur by
taining sodium sulfate (RH 95%). During the first 12 h, the samples saponification, which consists in the reaction between the base and
were weighed every hour; then, they were weighed every 12 h until the lipid, to cleave the ester bond and to form an organic salt and an
equilibrium was reached. This assay was performed in triplicate. alcohol (Gunstone & Norris, 2013). The AS method provided starch
The water uptake was calculated by using the following equation with the lowest content of lipids and ash, indicating that acid pH
(Equation (3)): allowed ash and lipids to solubilize and hydrolyzed the ester bond
of lipids, to generate fatty acid and alcohol (Allinger, 1976).
Mt  MO The babassu mesocarp flour and the starch isolated by WS dis-
Water uptake ¼  100 (3)
MO played similar content of amylose, which was higher than the
content of amylose in the starches isolated by KS and AS. More
where Mt is the weight of the film at time t, and Mo corresponds to intense leaching/degradation of amylose in alkaline and acid pH
the weight of the dry film determined after drying overnight at could account for this observation. According to Karim et al. (2008),
105  C (before exposure to 95% RH). alkaline and acid media may hydrolyze the structures of starch by
386 B.C. Maniglia et al. / Food Hydrocolloids 70 (2017) 383e391

Table 1
Centesimal composition of babassu mesocarp flour and starches (WS, KS and AS) obtained by the starch isolation processes (g/100 g of dry material).

Material Moisture* Ashes Lipid Protein Fiber Starch Amylose Yield

(g/100 g starch)

Babassu mesocarp 10.53 ± 0.43b 1.04 ± 0.11a 1.51 ± 0.04a 1.77 ± 0.06a 11.11 ± 0.42a 84.57 ± 0.44d 37.93 ± 1.04a e
WS1 15.09 ± 1.65a 1.13 ± 0.12a 1.75 ± 0.36a 1.38 ± 0.01b 3.70 ± 0.20b 92.04 ± 0.43c 36.56 ± 0.49a 65 ± 3c
KS1 14.80 ± 1.20a 1.12 ± 0.03a 0.13 ± 0.03b 1.16 ± 0.02c 0.59 ± 0.08d 97.00 ± 0.24a 24.82 ± 0.17b 85 ± 2a
AS 10.73 ± 0.32b 0.29 ± 0.07b 0.08 ± 0.02b 1.36 ± 0.10b 2.98 ± 0.19c 95.29 ± 0.23b 21.29 ± 0.96c 72 ± 2b

*Expressed on moisture basis; S: starch (obtained by difference) ¼ (100 e (Ashes (%) þ Lipid (%) þ Protein (%) þ (Food Fiber (%)).
Results also shown in the work of Maniglia and Tapia-Bl acido (2016).
AeD: different small caps in the same column indicate significant difference between the babassu mesocarp and the starches, as revealed by Tukey test, p < 0.05.

preferentially attacking the amorphous region of the granule evident. The films were easily removed from the mold without
(which corresponds mainly to amylose polymer), to leach/degrade signs of a sticky characteristic. However, the flour film displayed
these structures. The lower content of lipids of the KS and AS non-homogenous structure in which agglomerates emerged,
starches could also contribute to this effect: fewer amylose-lipid whereas the starch films exhibited a homogeneous matrix.
complexes should exist in these starches, conferring less protec- Table 2 shows that the flour films were more opaque than the
tion to the structure of starch undergoing alkali or acid attack starch films. The presence of a major quantity of lipids, proteins,
(Wang & Copeland, 2015). The AS method yielded starch with the and fibers in the babassu mesocarp flour must have reduced the
lowest content of amylose because the hydrogen ions from the acid transparency of the flour film. These components may have
solution may have penetrated behind the helix double structures of agglomerated in the film matrix, to generate the dark spots (seen in
starch to a greater extent than the hydroxyl ions from the alkaline Fig. 1). Pelissari et al. (2013) observed this same behavior when they
solution, culminating in higher rupture of the amylose polymers compared banana starch films and banana flour films (29.5 and
(Nakazawa & Wang, 2004). 51.3%). Daudt et al. (2016) also verified this behavior when they
analyzed pinh~ ao starch and flour films (8.5 and 10.3%).
The method used to isolate the babassu starch also influenced
3.2. Visual aspect and optical properties of the babassu films
the luminosity (L*), redness (a*), yellowness (b*), color difference
(DE), and opacity of the starch films (Table 2). The starch isolated by
Fig. 1 depicts the visual aspect of the babassu mesocarp flour
KS gave the darkest (lower L* value), most colorful, and most red-
film (flour film) and of the babassu mesocarp starch films (WS, KS,
dish (higher a* value) film (see Fig. 1) due to oxidation of the
and AS starch films). In general, the babassu films had good
phenolic compounds associated with the chromophore groups
appearance and transparency; no fractures or grooves were

Fig. 1. Visual aspect of the films prepared with babassu mesocarp flour and starch (WS, KS, and AS).
B.C. Maniglia et al. / Food Hydrocolloids 70 (2017) 383e391 387

Table 2
Parameters of color (L*, a*, and b*), color difference (DE), and opacity for babassu mesocarp flour and starch (WS, KS and AS) films.

Films L* a* b* DE* Opacity


Flour 73.24 ± 0.55c 5.25 ± 0.33c 23.27 ± 0.19c 30.41 ± 0.46c 6.23 ± 0.03a
WS 75.70 ± 0.10b 7.58 ± 0.23b 29.53 ± 0.20b 34.31 ± 0.32b 5.69 ± 0.03c
KS 71.08 ± 0.12d 15.38 ± 0.18a 32.73 ± 0.43a 41.77 ± 0.48a 5.81 ± 0.07b
AS 81.29 ± 0.49a 3.82 ± 0.23d 20.01 ± 0.72d 22.46 ± 0.89d 4.09 ± 0.23d

aed: different small caps in the same column indicate significant difference between films with different matrixes (babassu mesocarp flour or starches), as revealed by Tukey's
test, p < 0.05.

(Oliveira, 2015). The opposite effect occurred for the AS starch film, antioxidant activity of the starch films decreased only slightly. The
which displayed higher luminosity and smaller color difference and phenolic compounds may have been lost due to oxidation of the
opacity as compared to the other films produced herein. Acid me- phenolic groups by the heating applied during preparation of the
dium may have decreased the number of chromophore groups and filmogenic solution and during the film drying process.
the oxidation of phenolic compounds, resulting in a less colorful On the other hand, the flour film had higher content of total
starch (Terci & Rossi, 2002). phenolic compounds as compared to the starch films even though
all the babassu films showed high antioxidant activity ranging from
3.3. Total phenolic content and antioxidant activity 63.4 to 72.3%. This activity was greater than the antioxidant activity
of turmeric flour films (Maniglia, De Paula, Domingos, & Tapia-
Table 3 lists the contents of total phenolic compounds and the cido, 2015).
antioxidant activity, measured by the DPPH method, of the initial
materials (babassu mesocarp flour and starches obtained by the 3.4. Mechanical properties of the films
WS, KS, and AS methods) and of the films produced with these
materials. The isolation methods decreased the content of total Table 4 summarizes the mechanical properties of the flour, WS
phenolic compounds in the starches as compared to the babassu starch, KS starch, and AS starch films. The starch films were more
mesocarp flour. However, this isolation process did not alter the resistant, more rigid, and less elongable than the flour film. Because
antioxidant activity of the starches. Probably, a small amount of the flour had higher contents of fibers, lipids, and proteins than the
phenolic compounds sufficed to provide the antioxidant activity or, starches, these structures may have disrupted the network in the
as mentioned by Maniglia and Tapia-Bla cido (2016), the presence of flour film matrix, decreasing the rigidity of the truss-like three-
other unknown structures could contribute to the antioxidant ac- dimensional structure and giving less mechanically resistant films
tivity. The AS method yielded the starch and starch films with the n, 2012). On the other hand, the starch must have
(Marcilla & Beltra
highest content of total phenolic compounds as compared to all the contained more amylose-amylose, amylopectin-amylopectin, and
babassu materials investigated herein. This behavior could be amylose-amylopectin interactions due to its higher purity grade
associated with the ascorbic acid used to isolate the babassu starch: (Mali, Grossmann, & Yamashita, 2010). The WS starch yielded more
this acid acted as an antioxidant agent and prevented the oxidation mechanically resistant, more rigid (high values of tensile strength
of phenolic compounds and of other agents that were prone to and Young's modulus), and less flexible (low elongation at break
oxidation (Oetari, Sudibyo, Commandeur, Samhoedi, & Vermeulen, values) films as compared to the KS and AS starches due to its high
1996). Meanwhile the KS starch and its film had the lowest content content of amylose. The content of amylose is important for gel
of total phenolic compounds, but these materials also showed formation and subsequent generation of the films because the
antioxidant activity. According to Oliveira (2015), alkaline medium linear structure of amylose allows the molecules to orient parallel
may have decreased the content of total phenolic compounds to each other, which favors the formation of hydrogen bonds be-
because it favored formation of phenoxides from phenolic com- tween the hydroxyl groups of adjacent polymers and gives rise to
pounds associated with chromophore groups. films with higher crystallinity (Tako, Tamaki, Teruya, & Takeda,
Comparison of the initial materials and the prepared films 2014). The flour film was slightly more flexible than the starch
showed that the process of film production caused loss of phenolic films (2.85% as compared to 0.68e2.01%, respectively). This differ-
compoundsd30%, 20%, 40%, and 25% for the flour film, WS starch ence might have arisen from the major content of lipids in the
film, KS starch film, and AS starch film, respectively. However, the babassu flour, which could act as plasticizer and diminish the

Table 3
Total phenolic content and antioxidant activity determined by the DPPH method for the initial materials (babassu mesocarp flour and starches obtained by WS, KS, and AS) and
the films produced with these materials.

Material Total phenolic Antioxidant activity

(mg GAE/100 g of film) (%)

Flour Material 98.3 ± 2.3aA 63.4 ± 1.5cA

Films 68.2 ± 3.0aB 63.4 ± 0.9bA
WS Material 63.7 ± 3.1cA 66.8 ± 2.1bA
Films 50.7 ± 1.6cB 63.8 ± 1.0bA
KS Material 8.2 ± 0.1dA 68.7 ± 1.0bA
Films 5.0 ± 0.9dB 64.9 ± 1.3bB
AS Material 77.0 ± 2.0bA 72.3 ± 0.9aA
Films 57.2 ± 1.1bB 70.0 ± 1.4aA

aed: different small caps in the same column indicate significant difference between different materials or between different films, as revealed by Tukey's test, p < 0.05.
A - B: different big caps in the same column indicate significant difference between the material and the film produced with the same material, as revealed by Tukey's test,
p < 0.05.
388 B.C. Maniglia et al. / Food Hydrocolloids 70 (2017) 383e391

Table 4
Mechanical properties of babassu mesocarp flour and starch (WS, KS and AS) films.

Films Thickness Tensile Strength (MPa) Elongation at break (%) Young's Modulus (MPa)

Flour 80 ± 5a 12.50 ± 1.23c 2.85 ± 0.16a 483.80 ± 135.97c

WS 88 ± 3a 63.00 ± 4.09a 0.68 ± 0.18c 4285.9 ± 208.76a
KS 82 ± 11a 26.72 ± 2.91b 2.01 ± 0.08b 1954.74 ± 267.05b
AS 77 ± 9a 24.46 ± 2.89b 1.94 ± 0.17b 1870.60 ± 195.02b

aec: different small caps in the same line indicate significant difference between films with different matrixes (babassu mesocarp flour or starches), as revealed by Tukey's test,
p < 0.05.

relative number of polymerepolymer interactions while increasing available to interact with water molecules (Wurzburg, 1986, p. 277).
n, 2012). The babassu starch films
the flexibility (Marcilla & Beltra Concerning the content of amylopectin, Li, Shoemaker, Ma, Shen,
produced in this work were more resistant and rigid and less and Zhong (2008) stated that amylopectin films are more hydro-
flexible than pinha~o starch films plasticized with glycerol (20 g of philic than amylose films. Hence, the fact that the KS and AS
plasticizer/100 g of starch, tensile strength: 18.56 MPa, Young's starches had a major content of amylopectin also contributed to the
modulus: 1025 MPa, and elongation at break: 2.8%) (Daudt et al., formation of a more hydrophilic film. Because water can diffuse
2016). On the other hand, the babassu flour films were more me- more easily through films that are rich in amylopectin (Mehyar &
chanically resistant and more flexible than turmeric flour films Han, 2004; Stading, Hermansson, & Gatenholm, 1998), the KS and
plasticized with 22% glycerol (8.88 MPa and 1.97%) (Maniglia et al., AS starch films were more permeable to water vapor than the WS
2015). starch film. The network formed in materials rich in amylose (a
more linear polymer), like the WS starch, has more closely packed
polymers, which resulted in smaller pores as compared to matrixes
3.5. Functional properties of the films bearing more amylopectin polymers (more branched), such as the
AS and KS starches. In addition, amylopectin is more hydrophilic
The flour film presented higher solubility, higher WVP, and lower than amylose, which should culminate in higher interaction be-
value of contact angle than the starch films (Table 5). Hence, the tween amylopectin and water and facilitate diffusion of water
flour film was more hydrophilic than the starch films. The presence molecules in the case of the KS and AS starch films (Li et al., 2008).
of more hydrophilic groups from proteins and soluble fibers present The solubility of babassu films ranged from 24.3 to 39.0%.
in major quantity in the flour may have led to a greater number of Therefore, these films were less soluble than amaranth flour and
interactions between the flour components and water molecules amaranth starch films (solubility ¼ 42.3 and 62.5%, respectively)
(Pelissari et al., 2013), making the flour film more soluble and (Tapia-Bl
acido, Sobral, & Menegalli, 2005), but they were more
permeable to water vapor than the starch films. In addition, the less soluble than quinoa flour and quinoa starch films (18.7 and 15.9%,
homogeneous and more agglomerated structure of the flour film respectively) (Araújo-Farro, Podadera, Sobral, & Menegalli, 2010).
may have created pores, thereby allowing more paths for water to The WVP values of the babassu films produced in this work were
diffuse through the film and increasing the value of WVP (Martin- greater than the WVP of the achira flour and achira starch films (0.7
Polo, Mauguin, & Voilley, 1992). Daudt et al. (2016) verified a and 2.7  1010 g/m.s.Pa, respectively) produced by Andrade-
similar behavior for pinh~ ao starch (WVP ¼ 3.11  1010 g/m.s.Pa) Mahecha, Tapia-Bla cido & Menegalli (2012).
and flour films (WVP ¼ 3.75  1010 g/m.s.Pa), and Dias et al. (2010)
verified a similar behavior for rice starch films (WVP ¼ 0.5  1010 g/
3.6. Water uptake of the films
m.s.Pa) and rice flour films (WVP ¼ 1.1  1010 g/m.s.Pa).
In relation to the starch films, Table 5 shows that the KS and AS
Fig. 2 illustrates water uptake by the flour and WS, KS, and AS
methods gave starch films with higher content of moisture, higher
starch films plasticized with glycerol. All the babassu films behaved
solubility, higher WVP, and lower value of contact angle than the
similarly: they rapidly absorbed water up to 24 h. Water absorption
WS method. Therefore, the starch isolated by AS and KS yielded
slowed thereafter, until it became constant at 170 h.
more hydrophilic films than the starch isolated by WS. This could
The water uptake behavior of the babassu films demonstrated
be justified by the contents of amylose and amylopectin in the
different starches. First, the KS and AS starches had lower content of
amylose as compared to the WS starch. Starches with lower content
of amylose form a less linear network in the matrix, with fewer
interactions between the polymers. Consequently, more sites are

Table 5
Functional Properties (Moisture, solubility, WVP, and contact angle) of babassu
mesocarp flour and starch (WS, KS and AS) films.

Films Moisture Solubility WVP Contact Angle

(%) (%) (1010 g/m.s.Pa) ( )

Flour 11.82 ± 0.23a 39.02 ± 0.31a 9.30 ± 0.30a 56 ± 1d

WS 7.33 ± 0.21c 24.32 ± 0.78d 3.52 ± 0.20c 73 ± 3a
KS 11.13 ± 0.22b 34.65 ± 0.98c 5.12 ± 0.62b 63 ± 1b
AS 11.56 ± 0.11a 37.02 ± 0.48b 5.52 ± 0.30b 60 ± 1c

WVP: Water vapor permeability.

a - d: different small caps in the same line indicate significant difference between
films with different matrixes (babassu mesocarp flour or starches), as revealed by Fig. 2. Water uptake by the films prepared with different matrixes (babassu mesocarp
Tukey's test, p < 0.05. flour and starches WS, KS, and AS).
B.C. Maniglia et al. / Food Hydrocolloids 70 (2017) 383e391 389

that the starch films were less hydrophilic than the flour film,
which agreed with the functional properties summarized in
Table 5. Although the babassu flour had higher amylose content
than the babassu starches (WS, KS, and AS), the flour film displayed
higher water uptake capacity due to its high contents of proteins,
fibers, and total phenolic compounds. Regarding the starch films,
Fig. 2 demonstrated that the AS starch film presented higher water
uptake capacity as compared to the KS and WS starch films. This
behavior could be related to the lower content of amylose and to
the higher content of amylopectin of the AS starch, which led to
greater affinity for water (Li et al., 2008). The WS starch yielded
films with the lowest water uptake capacity. In general, the babassu
films produced in this study had high water uptake capacity
(35e48%); therefore, these films cannot be used as packaging for
foods with high water activity (Mali et al., 2010).

3.7. Microstructure of the films

Fig. 4. X-ray diffraction patterns of babassu mesocarp flour and starch (WS, KS, and
AS) films with the respective crystallinity index.
Fig. 3 displays the SEM micrographs of the surfaces and cross-
sections of the babassu flour and starch (WS, KS, and AS) films.
The surface of the flour film was less homogeneous and contained their high WVP (Table 5).
more imperfections as compared to the surface of the starch films.
These irregularities on the surface may be responsible for low
mechanical resistance of flour films. 3.8. X-ray diffraction (XRD) of the films
Regarding the starch films, although the WS starch was less pure
than the other starches, its higher content of amylose may have Fig. 4 brings the XRD patterns of the flour and starch (WS, KS,
promoted the formation of a more organized network. Hence, and AS) films with the respective crystallinity index. All the starch
macromolecules were better distributed in this starch than in the films displayed peaks at 15, 17, 19, and 22 respective (2q), which
AS and KS starches, which resulted in a more homogenous matrix are characteristic of starch type B. However, a peak appeared at 5.6
and consequently generated a more mechanically resistant film in the XRD patterns of the KS and WS starch films, and a peak
(Table 4). The cross-section of the WS starch film was the densest. emerged at 12 in the XRD pattern of the WS starch film. The peak
However, the flour and the KS and AS starch films had more at 5.6 is only present in B-type starches, and the peak at 12 are
laminated structure with small cracks, which could account for typical of starch A-type. Thus, the WS starch film showed a typical

Fig. 3. Scanning electron micrographs of the surfaces and cross-sections of the films prepared with babassu mesocarp flour or starches (WS, KS, and AS). Magnification of 500.
390 B.C. Maniglia et al. / Food Hydrocolloids 70 (2017) 383e391

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Machado, A. E. H., Furuyama, A. M., Falone, S. Z., Ruggiero, R., da Silva Perez, D., &
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Estado de Sa~o Paulo (Sa~o Paulo Research Support Foundation using titanium dioxide: The role of the hydroxyl radical. Chemosphere, 40(1),
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Mali, S., Grossmann, M. V. E., & Yamashita, F. (2010). Filmes de amido: Produça ~o,
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