Application of Gum Arabic and Maltodextrin For Encapsulation of

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International Journal of Biological Macromolecules 140 (2019) 59–68

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International Journal of Biological Macromolecules

journal homepage: http://www.elsevier.com/locate/ijbiomac

Application of gum Arabic and maltodextrin for encapsulation of


eggplant peel extract as a natural antioxidant and color source
Khashayar Sarabandi, Seid Mahdi Jafari ⁎, Alireza Sadeghi Mahoonak, Adeleh Mohammadi
Faculty of Food Science & Technology, Gorgan University of Agricultural Sciences and Natural Resources, Gorgan, Iran

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

Article history: Our aim was to produce an encapsulated powder loaded with eggplant peel extract as a natural source of color
Received 6 March 2019 and antioxidants through gum Arabic and maltodextrin. The effect of spray drying inlet temperature (140–170
Received in revised form 13 August 2019 °C) and various carriers (maltodextrin, gum Arabic, and their combination) on powder production yield, physical
Accepted 15 August 2019
properties, flowability, color, total phenolic content (TPC), antioxidant activity, infrared spectroscopy (FTIR), mi-
Available online 15 August 2019
crostructure and particle size were investigated. Our results revealed that physicochemical properties of powders
Keywords:
were influenced by the carrier type and inlet temperature. Obtained powders by maltodextrin at 170 °C showed
Microencapsulation the highest TPC (5.2 mg/g), DPPH (73.4%), ABTS (90.5%), TEAC (2. 5 mM), hydroxyl radicals scavenging activity
Eggplant peel extract (79.1%) and reducing power (1.2 Abs700) among all samples. FTIR spectroscopy indicated that the extract was en-
Antioxidant activity capsulated by the carriers. Microstructure evaluation of powders showed some hollow particles with matrix-type
structures. Sensory evaluation indicated that addition of encapsulated eggplant extract into the formulation of
gummy candy improved its color and overall acceptability.
© 2019 Elsevier B.V. All rights reserved.

1. Introduction However, phenolics and anthocyanins of the plant extracts are sen-
sitive to environmental and processing stresses such as heat, light, and
By-products and wastes are producing in food factories every day. oxygen [7]. An effective strategy to overcome this problem is applying
Most of them are a rich source of bioactive compounds, which lead to microencapsulation. There are many different microencapsulation
the increasing attention of researchers and companies for the extrac- methods for bioactive compounds including spray-drying, liposome en-
tion, investigation, and their application in food products [1]. trapment, inclusion complexation, coacervation, co-crystallization,
Balasundram et al. [2] reviewed some studies about by-product results freeze-drying, and emulsification [8]. Among them, spray-drying is an
from plant-based food processing and reported that there were a lot industrial, economical, and flexible method which is commonly used
of by-products rich in phenolic compounds including rice hulls, almond to transform the liquid products into dry powders [9]. In this method,
hulls, buckwheat hulls, pistachio hulls, olive industry pomace, lemon the sensitive compounds are covered within the carrier material,
peel, peach, apple, orange, grapefruit, banana, and also seeds and skin which leads to their protection against environmental stresses [10].
of grape and tomato. Eggplant (Solanum melongena) is mainly produced Many properties of encapsulated powders such as encapsulation ef-
by Asian and Mediterranean countries and contains biologically impor- ficiency depend on the type and characterization of carrier material; so,
tant ingredients such as phenolic compounds, minerals, and various vi- choosing the correct wall material is the main step to produce efficient
tamins including vitamin C [3]. The peel of eggplant is one of the by- encapsulated powders. Maltodextrin and gum Arabic due to their high
products in the food industry and is a rich source of different phyto- solubility, good biocompatibility, optimum viscosity, and safety are
chemicals with antioxidant activity such as anthocyanins, especially among the most commonly materials which have been used as carriers
delphinidin 3-rutinoside (tulipanin) and delphinidin 3-(p-coumaroyl for the spray-drying encapsulation of bioactive compounds [10,11]. For
rutinoside)-5-glucoside (nasunin) [4]. These properties have made it example, maltodextrin has been used for the encapsulation of bayberry
possible to use the eggplant peel extract as a good source of natural polyphenols [12], Sumac extract [13], casein hydrolysates [14], and
colors with health advantages in food formulations [5]. Hence, some re- pomegranate peel extract [15]. Gum Arabic alone or combined with
searchers evaluated the effect of various treatments and solvents on the maltodextrin has also been used for encapsulation of grape polyphenols
extraction of colored compounds and anthocyanins from the eggplant [11], sour cherry juice [16], mountain tea water extract [17], pomegran-
peel [6]. ate juice [18], saffron petal anthocyanins [19], saffron extract [20], and
barberry anthocyanins [21,22]. These results showed the all of product
⁎ Corresponding author. properties were influenced by spray-drying parameters such as drying
E-mail address: [email protected] (S.M. Jafari). air temperature and carrier's type and combination.

https://doi.org/10.1016/j.ijbiomac.2019.08.133
0141-8130/© 2019 Elsevier B.V. All rights reserved.
60 K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68

To the best of our knowledge, there is no studies' dealing with phys- pump with a flow rate of 3 L/h. It was equipped with a rotary atomizer
icochemical properties of the spray-dried encapsulated eggplant peel (5 cm diameter) working by compressed air. Controlled parameters se-
extract. Also, fortification of gummy candy with microencapsulated lected as feed temperature (25 ± 1 °C); atomizer pressure (4.5 ±
eggplant peel extract as a natural color and antioxidant source has not 0.1 bar); atomizer rotational speed (18,000 rpm); and the feed flow
been studied. Therefore, the aims of this study were 1) spray-drying en- rate (15 mL/min) according to our previous studies [16]. A co-current
capsulation of eggplant peel extract using maltodextrin, gum Arabic or flow of pre-prepared feed solutions and inlet air (140 and 170 °C) was
both at inlet temperatures of 140and 170 °C, and 2) fortification of used in the system. The collected powders were transferred into the
gummy candy as a food model system with the microencapsulated egg- desiccator to reach a constant temperature and prevent moisture
plant peel extract and investigation of the sensory properties of final changes, and then stored in dark bottles for further analysis.
products.
2.3. Analysis of encapsulated powder properties
2. Materials and methods
2.3.1. Production yield
2.1. Materials Production yield of the spray-drying process was determined as the
mass percentage of final product compared to the mass of total solids
Maltodextrin (Pooran powder, Isfahan, Iran) and gum Arabic measured in the feed solution.
(Samchon Chemical, Korea) were used as carrier agents. Maltodextrin
had a Dextrose Equivalent (DE) = 18–20, with a molecular weight of 2.3.2. Moisture content
1925 ± 96 (g/mol) and a degree of polymerization = 2–20 (units of Precisely weighed 2 g of powders were taken in a formerly dried and
glucose). Arabic Gum (Acacia senegal, molecular mass ∼380,000) as a weighed Petri dish, and then placed in the oven (2–3 h at 105 ± 2 °C) till
complex blend of natural polysaccharides was composed of three com- reaching a stable weight. The amount of moisture was calculated based
ponents differing in molecular size and protein content namely on the loss in weight before and after drying [23].
arabinogalactans (AG), arabinogalactan proteins (AGP), and glycopro-
teins (GP). The chemicals used in this research, including Folin– 2.3.3. Solubility and wettability
Ciocalteu reagent, gallic acid, 1,1-Diphenyl-2-picrylhydrazyl (DPPH), Approximately 1 g of each powder sample was added to 100 mL dis-
2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) diammonium tilled water and stirred using a magnetic stirrer (400 rpm for 4 min).
salt (ABTS), 6-hydroxy-2,5,7,8-tetramethychroman-2-carboxylic acid The produced solution was centrifuged at 4000 ×g for 4 min. A 25 mL al-
(Trolox), sodium carbonate, and thiobarbituric acid (TBA) were pur- iquot of the supernatant was transferred to a pre-weighted Petri dish
chased from Sigma–Aldrich; α-deoxyribose was purchased from Fluka and dried in an oven at 105 °C for 5 h. The weight of dried supernatant
(Stockholm, Sweden), potassium persulphate, trichloroacetic acid as a percentage of the original powder was used to determine the solu-
(TCA), and ferric chloride were purchased from Merck (Darmstadt, bility in water [24].
Germany). Other chemicals were of analytical grade. Wettability of powders was calculated according to the method of
Botrel et al. [25]. Briefly, 0.1 g g of each sample was sprinkled over the
2.2. Methods surface of 100 mL distilled water at room temperature without agita-
tion. The time was recorded for the particles to become completely
2.2.1. Preparation of eggplant peel extract submerged.
The fresh eggplant was purchased from a local market in Gorgan,
Iran. The eggplant peels were removed using a sharp knife and were 2.3.4. Hygroscopicity
dried at room temperature in the shadow for 3 days. Then, the dried For hygroscopicity measurements, 1 g of each spray-dried powder
peels were ground, sieved (40 mesh), and stored at −18 °C for extrac- was transferred into a desiccator with saturated NaCl solution at 25 °C
tion. The eggplant peel extracts were obtained by the following extrac- for 7 days (RH = 75%). Then, the samples were weighed, and hygro-
tion conditions: 5 g of powdered eggplant peel was mixed with 100 mL scopicity was reported as g of adsorbed moisture per 100 g dry powder
distilled water, and kept in a water bath (WNB22, Memmert, Germany) and expressed as percentage [26].
at 80 °C for 40 min. The temperature and time of extraction process
were selected based on trial and error. Higher temperatures reduced 2.3.5. Bulk density and tapped density
the amount of total phenolics and antioxidant activity of the extract. To determine the bulk density, 2 g of powders were transferred into
The color of extract was similar to the skin color of eggplant. The pres- a 10 mL graduated cylinder. The bulk density was calculated as the ratio
ence of violet color can be attributed to the existence of numerous com- of mass to the volume occupied in the cylinder (g/mL). The tapped den-
pounds in the skin of eggplant. But, after using citric acid (in the sity was determined by tapping the cylinder (an average of 100 taps).
formulation of gummy candy) and reducing the pH of extract, the The final volume was read and used to calculate the tapped density [27].
color of anthocyanin compounds predominated and the color of extract
was red. Then, the obtained extract was centrifuged for 10 min at 5000 2.3.6. Flowability (cohesiveness, compressibility and angle of repose)
×g (514R, Cambi, Hanil science industrial, South Korea) and filtered 5 g of each powder was dumped on a flat horizontal surface from a
using Whatman filter paper No. 1; the filtrate was kept in the dark flasks constant height (10 cm) through a funnel with 10 mm outlet diameter,
at 4 °C for further use [13]. to form a cone. The angle formed between the side surface and the base
of a cone was measured and characterized as repose angle [28]. Cohe-
2.2.2. Encapsulation of eggplant peel extract by carbohydrate biopolymers siveness and compressibility of the powders were expressed as Hausner
Three careers including maltodextrin (MD), gum Arabic (GA), and ratio (HR = TD/BD) and Carr index (CI = 1 − 1/HR), respectively. In
their combination (1:1) were used as the encapsulating agent and dis- these equations, TD and BD are the tapped and bulk density, respec-
solved in the eggplant peel extract solution (10% w/v) under magnetic tively [29].
agitation (L-81, Labinco, Netherlands) for 30 min. Then, the prepared
feed solutions were kept for 3 h to complete hydration. For all runs, 2.3.7. Color analysis
300 mL of each feed solution (13% soluble solids content) was used for The color parameters of the spray-dried powders were measured by
spray-drying. L⁎, a⁎, and b⁎ indices. First, 3 g of each spray-dried sample was trans-
The drying process was done using a pilot-scale spray-dryer with the ferred into Petri dishes and placed into a box with white interior walls
main chamber of 1 m diameter, 2 m cylindrical height and a peristaltic (in dimensions of 50 × 60 × 60 cm) equipped with a fluorescent lamp
K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68 61

with white light (40 W, 220 V). Images of samples were then taken by thiobarbituric acid (1.0% TBA) was added. The mixture was heated in
Canon digital camera (Powershot A3400) and color analysis was per- boiling water for 15 min then cooled in ice and the absorbance was
formed using Image J software (http://imagej.net) as described by monitored at 532 nm. The percentage of hydroxyl radical scavenging ac-
Sarabandi et al. [16]. The hue angle and chroma were calculated using tivity was calculated on the same formula described for DPPH radical
the following formula: scavenging activity.

Hue ¼ tan−1 ðb  =aÞ ð1Þ


2.4.5. Reducing power
h i1=2 The reducing power of samples was evaluated based on the method
2
Chroma ¼ ðaÞ2 þ ðbÞ ð2Þ of Ahmadi et al. [33]. 0.5 mL dissolved sample was added to 0.5 mL
phosphate buffer (0.2 M, pH = 6.6) and 0.5 mL of potassium ferricya-
nide (1%). The mixture was incubated in oven (50 °C for 30 min).
2.4. Measuring the phenolic content and antioxidant activity of encapsu- Then, 0.5 mL of 10% TCA was added to the solution and centrifuged at
lated powders 4000 ×g for 10 min. 1.0 mL of the supernatant was collected and
mixed with 1.0 mL distilled water and 0.2 mL of 0.1% ferric chloride;
To evaluate the phenolic content and antioxidant activity of samples, the absorbance was measured at 700 nm. An equal volume of distilled
1 g of each powder was dissolved in 10 mL distilled water and then, this water instead of the sample was used as blank.
solution was used for all experiments.
2.5. FTIR spectroscopy
2.4.1. Total phenolic content (TPC)
TPC was measured according to the method of Rafiee et al. [30] with The FTIR spectrum of pure maltodextrin, freeze-dried extract and
some modifications. Briefly, 40 μL of samples were mixed with 2.32 mL spray-dried extract with MD was performed with a FTIR Spectropho-
distilled water and 200 μL of Folin–Ciocalteu reagent. After 5 min, 600 μL tometer (Shimadzu 8400, Japan) using potassium bromide (KBr) discs
of Na2CO3 solution (20%) was added and the mixture was incubated at prepared from dried samples mixed with dry KBr (at a ratio of 1:100).
room temperature for 30 min. Then, absorbance was measured at Spectrum was recorded with a wavenumber range from 400 to
760 nm (PJ Instruments, model T80, England). Gallic acid was used as 4000 cm−1, and 16 scans per sample [34].
a standard for calibration curve.

2.4.2. DPPH radical scavenging activity 2.6. Microstructure analysis of powders


The DPPH radical scavenging activity of samples was evaluated ac-
cording to the method of Sarabandi et al. [26] with some modifications. The particle morphology of samples was evaluated by scanning elec-
Briefly, 100 μL of samples was mixed with 3.9 mL of ethanolic solution of tron microscopy (SEM) (HITACHI PS-230, Japan). A small amount of
DPPH (0.2 mM). The obtained mixture left at room temperature for each sample was attached to a double side adhesive tape fixed to
30 min in the dark, then centrifuged at 4000 ×g for 5 min. The absor- stubs, then coated with a thin layer of gold. Finally, the coated samples
bance was measured at 517 nm. Finally, the DPPH radical scavenging ac- were placed under the microscope (5 kV accelerating voltage) and the
tivity was measured using the subsequent formula: morphology of particles was observed.

I ð%Þ ¼ ðAbsc −Abss =Absc Þ  100 ð3Þ


2.7. Preparation and fortification of the gummy candy
In the above equation, Absc is the control absorbance (without the
sample) and Abss is the sample absorbance. Fortification of gummy candy was done with free extract (2%) and
different levels of microencapsulated samples (0.5–2% w/w). For the
2.4.3. ABTS+ radical scavenging activity manufacture of gummy candy, glucose syrup (32%), sugar (34%) and
ABTS+ radical scavenging activities of microencapsulated eggplant water were completely mixed and heated. Gelatin solution (9%) was
peel extract was calculated as reported by You et al. [31]. The ABTS+ so- prepared by dissolving the gelatin in boiling water (100 °C). Then, the
lution was prepared by mixing 7 mM ABTS+ stock solution with gelatin solution was added to the previously prepared solution and
2.45 mM potassium persulfate (1:1 v/v) and this mixture was kept at citric acid (0.4%) was added and mixed [35]. When the temperature of
ambient temperature for 14 h. Prior to the assay, the ABTS+ solution mixture decreased to 40 °C, the free and microencapsulated eggplant
was diluted with 0.2 M sodium phosphate-buffered saline (pH = 7.4) peel extract was added and gently mixed. The control sample was
until reaching to absorbance of 0.70 ± 0.01 at 734 nm. After that, 30 manufactured without the extract.
μL of dissolved powders was mixed with 3 mL of prepared ABTS+ solu-
tion. The mixture was vortexed (30 s) and 6 min stand in the dark place; 2.7.1. Sensory evaluation of produced gummy candies
then, the absorbance of samples was monitored at 734 nm. A standard Sensory evaluation was done by 18 semi-trained panelists with ages
curve was plotted by reacting 30 μL of Trolox at different concentrations between 20 and 30 (9 girls and 9 boys). 7-point Hedonic assessment
(50, 100, 250, 500, 750 and 1000 μM) with 3 mL of diluted ABTS+ solu- was used with the scores from 1 (very dislike) to 7 (very like). The sen-
tion. Results were reported as Trolox equivalent antioxidant capacity sory indices were considered for color, hardness, adhesiveness,
(TEAC, mM). chewiness, taste and overall acceptance [36].

2.4.4. Hydroxyl radical scavenging activity


Hydroxyl radical scavenging activity of the microencapsulated sam- 2.8. Statistical analysis
ples was determined based on Kim and Minamikawa [32] with some
modifications. The reaction mixture contained 0.5 mL of α- The obtained results were subjected to one-way analysis of variance
deoxyribose (10 mM), 0.9 mL of PBS (0.2 M, pH = 7.4), 0.2 mL of (ANOVA) using SPSS 19.0 software (SPSS Inc., Chicago, IL) for the deter-
FeSO4-EDTA (10 mM), 0.2 mL of hydrogen peroxide (10 mM) and mination of differences among samples. The results were reported as
mixed with 0.2 mL of each sample and incubated at 37 °C for 1 h. To the mean ± standard deviation (SD) and the means were compared
stop the reaction, 1.0 mL trichloroacetic acid (3% TCA) and 1.0 mL by the Duncan's multiple range tests within the 95% confidence interval.
62 K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68

3. Results and discussion The wettability time of spray-dried EPE was influenced by the type
of carrier (Table 1). Powders produced with MD showed the fastest wet-
3.1. Physicochemical properties of powders containing eggplant peel extract tability, but GA led to a significant decrease (P b 0.05) in the wettability
(EPE) rate of particles. The wettability values in the present study was shorter
than spray-dried sumac extract (1239 to 3263 s) prepared with MD at
3.1.1. Production yield different temperature of 160, 180, and 200 С° [13]. Various factors
Powder production yield is the most important indicator which such as wall materials, inlet temperature, moisture content, and particle
shows the efficiency of spray-drying process. Table 1 shows that the size affect the wettability of spray-dried powders. For example, Botrel
production yield of encapsulated EPE ranges from 39.58 to 66.47%. At et al. [25] reported that using only whey protein isolate, WPI (226 s)
the same inlet temperature, produced powders by maltodextrin (MD) showed the highest wettability time for fish oil powder compared to
showed higher powder recovery than derived samples from gum Arabic WPI/MD (130 s) and WPI/inulin (112 s). The powders with lower mois-
(GA). This can be related to increase in viscosity of the prepared feed so- ture content showed a high solubility and wettability. Also, wettability
lutions by GA, which leads to production of coarse droplets with a high time is inversely related to the particle size; large particles are able to
agglomeration. Tolun et al. [11] also revealed similar results with the easily dispersed into the water because there is a more space between
microencapsulated grape polyphenols extract using GA and MD. particles via a high porosity [27].
In this study, when the drying temperature increased from 140to
170 С°, the powder recovery, especially with MD increased from 3.1.4. Hygroscopicity
52.03% to 66.47%. This can be related to the better efficiency of heat Hygroscopicity is the ability of powders to absorb moisture from the
and mass transfer, faster water removal, and less stickiness of particles surrounding environment, which affects the physicochemical stability,
on the dryer walls when increasing the inlet temperature. Similar re- shelf life, and other parameters such as the flowability of spray-dried
sults have been reported by Tonon et al. [37] and Tolun et al. [11] who powders. In present study, hygroscopicity of powders was
worked with the spray-dried acai and grape polyphenol, respectively. 14.91–20.72% which was influenced by the inlet temperature and car-
However, Nadeem et al. [17] reported that increase in the drying tem- rier type (Table 1). The microencapsulated EPE produced by MD and
perature due to increased feed flow rate causes the production yield of GA showed the highest and lowest hygroscopicity, respectively. This
mountain tea powder to decline. can be attributed to the higher glass transition temperature of GA com-
pared to MD [20]. Also, increasing temperature from 140to 170 °C en-
3.1.2. Moisture content hanced the hygroscopicity of powders (P b 0.05) possibly due to
At the same inlet temperature, powders produced with GA pre- increase in the difference between humidity of compounds and envi-
sented higher moisture contents compared to MD (Table 1). This may ronment. In agreement with our results, a higher hygroscopicity of
be due to higher capacity of gums to maintain moisture compared to spray-dried powders containing grape polyphenols [11], and jamun
MD as starch derivative [17]. The moisture content was significantly in- fruit juice [27] was shown with increase in the inlet temperature. Hy-
fluenced by inlet temperature and it was decreased at higher tempera- groscopicity of the obtained powders in the present study was lower
tures (P b 0.05). In the elevated inlet temperature, heat transfer rate than amla juice powders, 46–56% [39].
within the atomized droplets/particles increases which leads to a
greater driving force for water evaporation and consequently, lower 3.1.5. Bulk and tapped density
moisture content of the samples [37]. In similar studies, decrease in Density of powders was affected by the inlet temperature and car-
the moisture content of mountain tea extract powder [17], acai powder riers type (Table 2A). The bulk and tapped density of powders produced
[37], olive pomace powder [38], sumac extract powder [13], amla juice by MD at an inlet temperature of 140 °C was 0.581 and 0.733 g/mL, re-
powder [39], and grape polyphenols powder [11] have been reported spectively; whereas they were decreased to 0.558 and 0.696 g/mL (P b
and attributed to increase in the spray-drying temperature. 0.05) by increasing temperature from 140to 170 °C. Higher drying tem-
peratures can decrease the density of powders by improving evapora-
3.1.3. Solubility and wettability tion rate, increasing the porosity of particles, decreasing wrinkles, and
Water solubility of powders loaded with EPE were between 94.31 producing large particles with a more porous structure. Similar findings
and 98.78% (Table 1) which was affected by the carrier type. Among were observed by Caliskan and Nur Dirim [13] who worked with sumac
all powders, those produced with MD showed a higher solubility than extract. Also, our results showed that the powder produced with GA had
GA-loaded samples (P b 0.05). Similar findings were observed by a lower density than MD. This can be attributed to the higher feed vis-
Sarabandi et al. [16], Wang and Zhou [40], Nadeem et al. [17] and cosity of GA compared to MD, which can produce larger particles [41].
Cano-Chauca et al. [24] who worked with sour cherry juice, soy sauce,
mountain tea and mango powder, respectively. Our results clearly 3.1.6. Flowability
showed that water solubility doesn't change with an increase in inlet Flowability is an important indicator which can be used to deter-
temperature. However, other studies reported that increase in the dry- mine the conditions of processing, mixing, filling, formulation, packag-
ing temperature led to a higher solubility of the mountain tea extract ing, and transportation of food and pharmaceutical powders. The high
powder [17], and jamun fruit juice powder [27]. value of flowability index indicates non-flowing of produced powders

Table 1
Production yield and physical properties of microencapsulated powders loaded with eggplant peel extract.

Treatments Production yield (%) Moisture content (%) Solubility (%) Wettability (Sec) Hygroscopicity (%)

MD 140 °С 52.03 ± 2.47b 3.57 ± 0.16b 98.27 ± 1.33ab 7.02 ± 1.04d 18.98 ± 0.29b
MD 170 °С 66.47 ± 3.64a 2.34 ± 0.22c 98.78 ± 0.53a 4.74 ± 1.13d 20.72 ± 0.38a
MD/GA 140 °С 47.25 ± 2.32b 3.74 ± 0.23ab 96.23 ± 0.64c 177.34 ± 13.14b 17.16 ± 0.28cd
MD/GA 170 °С 52.41 ± 2.85b 2.66 ± 0.19c 96.87 ± 0.41bc 112.36 ± 4.44c 17.94 ± 0.65c
GA 140 °С 39.58 ± 4.01c 4.11 ± 0.28a 94.31 ± 1.09d 284.08 ± 22.43a 14.91 ± 0.25e
GA 170 °С 48.74 ± 3.03b 2.68 ± 0.23c 95.55 ± 0.75cd 262.88 ± 16.33a 16.93 ± 0.74d

Data are presented as mean ± standard deviation (n = 3) and different letters in the same column indicate significant differences at the 5% level in Duncan's test.
MD: Maltodextrin; GA: Gum Arabic.
K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68 63

Table 2A
Density and flowability parameters of encapsulated powders containing eggplant peel extract.

Treatments Bulk density (g/mL) Tapped density (g/mL) Hausner ratio Carr index Angle of repose (°)

MD 140 °С 0.581 ± 0.014a 0.731 ± 0.015a 1.257 ± 0.006a 0.204 ± 0.003a 32.36 ± 1.48a
MD 170 °С 0.558 ± 0.015b 0.696 ± 0.016b 1.246 ± 0.016ab 0.197 ± 0.011ab 28.93 ± 2.02a
MD/GA 140 °С 0.545 ± 0.005b 0.674 ± 0.015bc 1.235 ± 0.026ab 0.190 ± 0.017ab 30.28 ± 2.71a
MD/GA 170 °С 0.537 ± 0.011bc 0.664 ± 0.014c 1.234 ± 0.008ab 0.189 ± 0.006ab 29.51 ± 2.09a
GA 140 °С 0.523 ± 0.006c 0.638 ± 0.007d 1.219 ± 0.018b 0.180 ± 0.013b 29.03 ± 1.51a
GA 170 °С 0.497 ± 0.011d 0.607 ± 0.006e 1.221 ± 0.024b 0.181 ± 0.016ab 28.94 ± 1.09a

Data are presented as mean ± standard deviation (n = 3) and different letters in the same column indicate significant differences at the 5% level in Duncan's test.
MD: Maltodextrin; GA: Gum Arabic.

[29]. In this study, only the spray-dried EPE produced with MD and GA 3.2. Total phenolic content and antioxidant activity of encapsulated
at 140С° showed significant differences in terms of the hausner ratio powders
(HR) and compressibility (Table 2A). This can be attributed to the differ-
ences in size and surface morphology of the particles, as well as low hy- Total phenolic content (TPC) is one of the most important indices for
groscopicity of the powder produced with GA. The HR and evaluating the antioxidant capacity of various plant extracts. We found
compressibility values of our powders were lower than the spray- that TPC of EPE was between 4.57 and 5.22 mg/g powder. This index
dried jamun fruit juice (1.57 to 1.72 and 0.36 to 0.42) reported by varied depending on the carrier and inlet temperature (Table 3). In
Santhalakshmy et al. [27]. We found no differences among the repose the case of carriers, the highest amount of TPC was related to MD pow-
angle of produced samples. Also, the inlet temperature did not have ders (at 170°С). But, partial or complete replacement of MD with GA re-
any significant effect on the repose angle. However, in a study by duced TPC (P b 0.05). This can be attributed to better entrapment of
Moreira et al. [42], they showed an enhancing in flowability of acerola polyphenols in MD structure than GA. When comparing to other plant
pomace powder by increasing the carrier concentration and replace- extracts, microencapsulated EPE showed a higher content of phenolics
ment of MD with cashew tree gum. The reasons of these results could than powders containing bayberry juice, 2.9 mg/g [12], and sumac ex-
be attributed to lower moisture contents and decrease in liquid bridges tract, 1.5 mg/g [13], but lower compared to spray-dried pomegranate
formation between particles. peel extract, 95–105 mg/g [15], Cagaita fruit extract, 9.9–31.2 mg/g
[43], and olive pomace extract, 4.4–39.5 mg/g [38].
Nadeem et al. [17] and Daza et al. [43] reported an increase in TPC
3.1.7. Color results and proanthocyanidins of the spray-dried mountain tea extract and
Color is one of the most important indicators of product quality. The cagaita fruit extract powder by increasing the inlet temperature, respec-
color parameters L, a, b, chroma and hue angle for the powders are given tively. But, Tolun et al. [11] reported the polyphenol content of grape
in Table 2B. The spray-dried EPE produced by GA showed a higher L, a, b, pomace extract powder decreased when temperature increased from
and hue angle compared to samples produced with MD. This trend can 120 to 160°С then a reverse tendency found in phenolic at 180 °C.
be correlated with the inherent color of the GA which is yellow to red- They explained the polymerization of polyphenols at high temperatures
dish. Also, the color of spray-dried samples increased significantly as a result of an increase in TPC of the samples. Although it is possible to
after replacement of MD with GA (P b 0.05). In general, by using GA as form a film rapidly around particles at higher temperatures, hence more
microencapsulating agent, the produced powders lost their natural, polyphenols maintain within the structure of carriers.
specific and attractive color of EPE. Effect of carrier type and inlet temperature on DPPH radical scaveng-
However, increase in inlet temperature from 140to 170 °C led to de- ing capacity of microencapsulated EPE is presented in Table 3. DPPH free
creases in color and b values of powders produced with MD and GA. This radical inhibition activity for all samples varied between 55.48 and
implied that the color was influenced by process parameters such as 73.38%. Powders produced with MD showed a higher antioxidant activ-
inlet temperature, type and composition of carrier. This was in agree- ity than GA. Also, the highest ABTS+ radical scavenging activities
ment with the results of Santhalakshmy et al. [27] who reported that (90.54%) and TEAC values (2.45 mM) was observed for samples pre-
higher temperatures led to decrease in color, also an increase in L values pared by MD at 170 °С. The evaluation of hydroxyl radical scavenging
and hue angle of jamun fruit juice powder. In another study, Nadeem (67.75–79.51%) and reducing power (1.12–1.24) of the EPE-loaded
et al. [17], spray dried mountain tea extract by β-cyclodextrin, GA, and powders indicated the high antioxidant activity of these samples. The
MD at 145, 155, and 165 С° and reported that increase in the inlet tem- value of these indicators was also significantly influenced by the carrier
perature led to a decrease in L value, increase in b value, and the color of type (Table 3). Results of these tests also showed a higher ability of MD
powders get a little darker. Also, our samples produced with GA were compared to GA in the production of powders with a high antioxidant
found to be darker and more reddish compared to MD. activity.

Table 2B
Color characterization of encapsulated powders loaded with eggplant peel extract.

Treatments L⁎ a⁎ b⁎ Hue angle (°) Chroma

MD 140°С 22.38 ± 0.46d 7.71 ± 0.25d 2.48 ± 0.05d 17.89 ± 0.89c 8.09 ± 0.22d
MD 170°С 25.59 ± 1.14c 6.17 ± 0.15e 1.05 ± 0.04e 9.66 ± 0.45d 6.26 ± 0.14e
MD/GA 140°С 32.37 ± 0.99b 10.66 ± 0.18a 29.43 ± 0.54c 70.08 ± 0.65b 31.32 ± 0.45c
MD/GA 170°С 34.39 ± 0.33a 10.06 ± 0.46b 28.97 ± 0.41c 70.85 ± 1.05b 30.68 ± 0.26c
GA 140°С 33.34 ± 0.68ab 9.48 ± 0.33c 31.67 ± 0.34a 73.32 ± 0.39a 33.05 ± 0.41a
GA 170°С 34.61 ± 0.53a 9.15 ± 0.09c 30.73 ± 0.71b 73.41 ± 0.52a 32.06 ± 0.65b

Data are presented as mean ± standard deviation (n = 3) and different letters in the same column indicate significant differences at the 5% level in Duncan's test.
MD: Maltodextrin; GA: Gum Arabic.
64 K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68

Table 3
Antioxidant properties of microencapsulated powders containing eggplant peel extract.

Treatments TPC (mg GAE/g) DPPH (%) ABTS (%) TEAC (mM) Hydroxyl (%) Reducing power (Abs700)

MD 140 °С 5.03 ± 0.12b 71.25 ± 0.97b 88.97 ± 0.28b 2.41 ± 0.008b 77.04 ± 1.17ab 1.21 ± 0.009b
MD 170 °С 5.22 ± 0.08a 73.38 ± 1.03a 90.54 ± 0.22a 2.45 ± 0.007a 79.05 ± 2.76a 1.24 ± 0.004a
MD/GA 140 °С 4.77 ± 0.06c 63.52 ± 1.22c 87.86 ± 0.55c 2.38 ± 0.008cd 70.94 ± 0.98c 1.13 ± 0.007de
MD/GA 170 °С 4.87 ± 0.07c 65.39 ± 0.99c 88.40 ± 0.40bc 2.39 ± 0.004c 74.75 ± 0.86b 1.17 ± 0.008c
GA 140 °С 4.58 ± 0.09d 55.73 ± 1.42d 86.87 ± 0.39d 2.35 ± 0.006e 67.25 ± 2.04d 1.12 ± 0.006e
GA 170 °С 4.57 ± 0.04d 55.48 ± 0.97d 87.79 ± 0.22c 2.38 ± 0.006d 70.24 ± 0.96c 1.14 ± 0.007d

Data are presented as mean ± standard deviation (n = 3) and different letters in the same column indicate significant differences at the 5% level in Duncan's test.
TPC: Total phenolic content; DPPH: DPPH radical scavenging activity; ABTS: ABTS radical scavenging activity; TEAC: Trolox equivalent antioxidant capacity; Hydroxyl: Hydroxyl radical
scavenging activity; Reducing power: Reducing power activity.
MD: Maltodextrin; GA: Gum Arabic.

In general, we found a significant positive correlation between TPC In regions between 900 cm−1 to 1600 cm−1, as well, numerous
and antioxidant activity. Also, the type of carriers had a significant effect peaks were found pertaining to phenolic ingredients. For example, the
on TPC and antioxidant activity of spray-dried powders. In agreement, bond in 1604 cm−1 (in freeze-dried eggplant peel extract) predomi-
Nadeem et al. [17] reported that antioxidant activity of mountain tea nantly belongs to C_C bond vibrations of phenolic and aromatic ingre-
powders was associated with their TPC. In another study, increase in dients [46]. This peak was disappeared in spray-dried samples,
inlet temperature did not show any significant effect on the antioxidant indicating that the extract was covered by the carrier in the microencap-
activity of cagaita fruit extract powders, owing to the protection offered sulation process. Similar peaks were also found in 1600 cm−1 that was
by the carriers [43]. belonged to symmetric and asymmetric stretching vibrations of such in-
gredients as chlorogenic acid [47] and the peak in 1618 cm−1 wave-
length pertained to ring C\\C stretch of phenyl in polyphenols
3.3. FTIR spectroscopy results structure [48]. In the freeze-dried extract, the peak observed in
1263 cm−1 region is possibly relating to proanthocyanidins [49]. This
Considering the physicochemical and antioxidant results of the final peak was not observed in microencapsulated extract. Furthermore,
powders, the encapsulated samples with maltodextrin were selected for only one peak was observed in 1155 cm−1 domain of pure maltodextrin
further analysis of the process effect on the chemical structure. Fig. 1 and encapsulated extract in this study whereas two peaks were evi-
shows the FTIR spectrums in the range of 400–4000 cm−1 for freeze- denced in 1121 cm−1 and 1045 cm−1 regions in freeze-dried extract.
dried extract, pure maltodextrin and spray-dried extract with MD. In These changes signify the encapsulation of the bioactive ingredients in
all samples, the peaks existent in frequencies between 2800 cm−1 to the extract by maltodextrin in spray-drying process. Generally, all of
3700 cm−1 were predominantly found pertaining to hydrogen bonds the peaks found for maltodextrin were also observed in the spray-
(O\\H stretch), carboxylic acids and residual water [44]. Double peak dried sample. The results of this part indicated that the spray-drying
near 2900 cm−1 frequency of the freeze-dried extract was found sub- process does not lead to the creation of new bonds between maltodex-
stantially belonging to the symmetric and asymmetric stretching of trin and ingredients of the extract.
C\\H bond in methyl group. The bonds feature lower intensities in the
spray-dried samples. The peaks were observed in 1155 cm−1 (C\\O 3.4. Microstructure of spray-dried powders
stretch, C\\O\\H bending), 1017 cm−1 (angular deformation of _CH
and _CH2 bonds), 850 cm−1 (deformation of CH2 and C1\\H) and Fig. 2 shows the particle morphology of the encapsulated EPE ob-
701 cm−1 (structural state of the pyranose ring) frequencies in pure tained by different carriers and inlet temperatures. Powder particles
maltodextrin structure [45]. Moreover, the peaks in frequencies near showed a continuous wall; the absence of surface cracks while, irregular
1650 cm−1 in maltodextrin were found mainly related to hydrogen structures with shrinkage on the particle surface and relatively deep
bonds of carbohydrates –OH groups [44]. dents were observed. Also, agglomeration did not occur as a result of

Fig. 1. FTIR spectrometry of freeze-dried eggplant peel extract, maltodextrin and spray-dried extract with maltodextrin (MD).
K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68 65

Fig. 2. SEM micrographs of encapsulated powders loaded with eggplant peel extract produced with (a) MD at 140 °C, (b) MD at 170 °C, (c) MD – GA at 140 °C, (d) MD – GA at 170 °C (e), GA
at 140 °C, and (f) GA at 170 °C. MD: Maltodextrin; GA: Gum Arabic.

sticking particles together. The microcapsules prepared with MD GA counterparts (Fig. 2e–f). This may be due to the fast removal of mois-
(Fig. 2a–b) showed more wrinkles and dents on their surfaces than ture and rapid cooling of produced particles produced with MD [11].

Fig. 3. (a) Morphology of the encapsulated eggplant peel extract within carriers indicating a matrix-type structure, existence of pores in the particles wall and hollow capsules, and (b) the
average particle size of encapsulated eggplant peel extract. MD: Maltodextrin; GA: Gum Arabic.
66 K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68

Table 4
Sensory properties of the gummy candies fortified with free and microencapsulated (MD-170°С) eggplant peel extract.

Treatments Color Hardness Gumminess Chewiness Taste Overall acceptance

Control 4.67 ± 0.48d 4.61 ± 0.61bc 4.56 ± 0.51a 4.06 ± 0.64b 4.71 ± 0.46cd 4.33 ± 0.49c
2.0% Extract 4.72 ± 0.57d 4.38 ± 0.50c 4.11 ± 0.32b 4.28 ± 0.46ab 4.56 ± 0.51cd 4.28 ± 0.46c
0.5% Powder 5.11 ± 0.32c 4.94 ± 0.64ab 4.51 ± 0.71ab 4.67 ± 0.68a 4.83 ± 0.79bc 4.67 ± 0.59c
1.0% Powder 5.83 ± 0.51b 5.22 ± 0.55a 4.72 ± 0.57a 4.56 ± 0.62a 5.28 ± 0.46a 5.61 ± 0.50b
1.5% Powder 6.22 ± 0.55a 4.78 ± 0.43b 4.71 ± 0.66a 4.68 ± 0.77a 5.17 ± 0.71ab 6.33 ± 0.48a
2.0% Powder 4.83 ± 0.38cd 4.72 ± 0.46bc 4.39 ± 0.70ab 4.27 ± 0.46ab 4.33 ± 0.49d 4.56 ± 0.62c

Data are presented as mean ± standard deviation (n = 18) and different letters in the same column indicate significant differences at the 5% level in Duncan's test.
MD: Maltodextrin.

The holes on the surface of some particles indicates the existence of Table 4 presents the measured sensory parameters of candy fortified
hollow structures (void) in the dried particles (Fig. 3a). These hollow with free and different levels of microencapsulated EPE. Among the ef-
structures represent production of particles with a matrix-type struc- fective sensory indicators, color is the first indicator reflecting the qual-
ture. In these structures, the core material is uniformly dispersed ity of a product that attracts consumer's attention [50]. The color of
throughout a matrix at the perimeter of particles. This can be explained candies was significantly influenced by the concentration of EPE pow-
because most of coating and core materials are hydrophilic and they ex- der (Fig. 4, Table 4). Among the produced samples, fortified candy
pand and uniformly combine to form a film and membrane [10]. Similar with 1 and 1.5% powders got the highest score in terms of color. Use
hollow structures are shown in spray-dried casein [14] and flaxseed of EPE powder led to creating an attractive red color in the product.
protein [34] hydrolysates,. However, higher levels of powder induced an opaque and undesirable
Fig. 3b shows the effect of carrier and inlet temperature on the aver- color in the candy. The free extract and different EPE powder levels
age particle size. An increase in inlet temperature and replacing MD did not have any effect on hardness, gumminess, and chewiness of
with GA caused the average particle size increases from 50.27 to 65.64 candy, but the taste of product was affected by the high level of powder
μm. It can be attributed to a high feed viscosity of GA [21]. This behavior (2%), an astringency was felt and it led to decreased taste scores. How-
was similar to data reported by Paini et al. [38] in spray-drying of olive ever, panelists did not report any astringency perception and unpleas-
pomace; higher temperatures led to a higher porosity and lower bulk ant taste for the product prepared with 0–1.5% EPE powders, which
density. However, Mishra et al. [39] showed that size of amla juice pow- can be attributed mainly to the presence of carbohydrates (particularly
der at higher inlet temperature was smaller than those produced at low sucrose) in the formulation of gummy candy [15].
temperatures due to a rapid rate of drying and formation of smaller Carbohydrates and gelatin used in the gummy candy formulation
sized particles. mask the astringent taste caused by the phenolic compounds of EPE.
The overall acceptance of fortified candy showed that samples with
3.5. Sensory evaluation of the fortified gummy candy with EPE 1.5% powder got the highest overall score. Some other studies have
evaluated use of food by-products as a source of fiber, phenolics, flavo-
The sensory evaluation is a critical factor which needs to be consid- noids and anthocyanins in various formulations, such as fortification of
ered for evaluating the ability of ingredients to fortify food formulations ice cream with microencapsulated pomegranate peel phenolics [15].
and acceptability of final products by consumers. In this study, powders The sensory scores indicated that the enriched candies (0.5% and 1.0%)
produced with MD (at 170 °C) were selected due to the preservation of could have a promising potential for market acceptance. In a study by
original natural color, high production yield, and the appropriate phys- Charoen et al. [35], enrichment of gummy jelly candy was carried out
ical and antioxidant properties for the fortification of the gummy candy. with antioxidant extract of Psidium guajava leaf and resulted in lower

Fig. 4. Effect of different ratios of spray-dried eggplant peel extract on the color of fortified gummy candies.
K. Sarabandi et al. / International Journal of Biological Macromolecules 140 (2019) 59–68 67

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