International Journal of Biological Macromolecules 152 (2020) 1125–1134

Contents lists available at ScienceDirect

International Journal of Biological Macromolecules

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

Microencapsulation of fingered citron extract with gum arabic, modified

starch, whey protein, and maltodextrin using spray drying
Amer Ali Mahdi a,b,c, Jalaleldeen Khaleel Mohammed a,b, Waleed Al-Ansi a,b,c, Abduljalil D.S. Ghaleb d,
Qais Ali Al-Maqtari a,c,e, Mengjiao Ma a,b, Mohamed Ismael Ahmed a, Hongxin Wang a,b,⇑
a
State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi, Jiangsu 214122, China
b
National Engineering Research Center for Functional Food, Jiangnan University, 1800 Lihu Road, Wuxi, Jiangsu 214122, China
c
Department of Food Science and Technology, Faculty of Agriculture, Sana’a University, Sana’a, Yemen
d
Faculty of Applied and Medical Science, Al-Razi University, Al-Rebatt St., Sana’a, Yemen
e
Department of Biology, Faculty of Science, Sana’a University, Sana’a, Yemen

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

Article history: The aim of this study was to investigate the characteristics of the Fingered citron extract (FCE) microcap-
Received 15 September 2019 sules powders with different formulations of the encapsulation carrier agents [gum arabic (GA),
Received in revised form 22 October 2019 maltodextrin (MD), modified starch (MS), and whey protein (WP)], which are obtained through spray
Accepted 23 October 2019
drying. Encapsulation yield, encapsulation efficiency, moisture content, hygroscopicity, water activity,
Available online 18 November 2019
density properties, Carr’s index, cohesiveness, flowability, porosity, wettability, solubility, color, particle
size, thermal behavior, relative crystallinity, and micrographs were analyzed. Moreover, chemical
Keywords:
structure of the microcapsule powder was identified using Fourier transform infrared spectroscopy
Citrus medica L. var. sarcodactylis Swingle
Encapsulation
(FT-IR). Best results were achieved when Fingered citron extract was encapsulated using gum
Encapsulation carrier agents arabic/maltodextrin/modified starch (GMS) formulation as carrier agents, where it had the highest
Spray drying encapsulation yield (89.39%) and encapsulation efficiency (87.20%). Furthermore, it achieved the best
result in density properties, flowability, porosity, wettability, and relative crystallinity. These results have
shown that using gum arabic/maltodextrin/modified starch formulation was superior for production of
the Fingered citron extract microcapsules powders.
Ó 2019 Elsevier B.V. All rights reserved.

1. Introduction In recent years, the food industry recommends addition of func-

Fingered citron (Citrus medica L. var. sarcodactylis Swingle) is
classified in the Rutaceae family and is broadly cultivated in Asian
countries. Fingered citron is usually consumed as a functional fruit.
Because of its phenolic compound content, Fingered citron has
been widely used as a raw material for some traditional Chinese
medicines that are used to treat a number of chronic diseases [1].
Fingered citron may be considered as a good source of phenolic
compounds that own high antioxidant activity and thus can be
used as safe food additives or nutritional supplements.
Ultrasonic/microwave-assisted extraction can be used as a safe
technology that does not necessitate the use of harmful solvents
[2].
⇑ Corresponding author: State Key Laboratory of Food Science and Technology
(Jiangnan University), School of Food Science and Technology, 1800 Lihu Road,
Wuxi, Jiangsu 214122, China.
E-mail address: hxwang@jiangnan.edu.cn (H. Wang).
tional compounds in various food products, however these com-
pounds are highly susceptible to environmental alteration [3].
Incorporation of bioactive compounds in food products using
micro- and nano-delivery systems may offer extra health benefits.
Beyond basic nutrition, encapsulation may help in retaining health
protective properties of such functional compounds, thus improv-
ing their bioavailability, while enabling their controlled release and
target delivery [4].
Micro- and nanoencapsulation is an emerging technology in the
food field that potentially allows the improvement of food quality
and human health [4]. Encapsulation is a process that entraps sub-
stance (active agent) into another substance wall material produc-
ing particles in millimeter scale, micrometer (microencapsulation)
or nanometer (nanoencapsulation) [5].
Encapsulation has also been defined as a technology of packag-
ing solids, liquids, or gaseous materials in small capsules that
release their contents at controlled rates over prolonged periods
and under specific conditions [3]. Furthermore, encapsulation
may also serve to transform liquid ingredients into free-flowing

https://doi.org/10.1016/j.ijbiomac.2019.10.201
0141-8130/Ó 2019 Elsevier B.V. All rights reserved.
1126 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134

powders for the convenience of improved handling and incorpora-
tion into dry food systems [6].
Microencapsulation is a useful way to enhance the bioavailabil-
ity and stability of bioactive compounds and controlling the release
of the active agent, the main aim of encapsulation is to protect core
material from environmental effects, thereby increases shelf life of
product and control release of the core material [7].
There are several types of encapsulation technique, such as a
centrifugal extrusion, vibrational nozzle, co-crystallization, freeze
drying, and spray drying. The most regularly used technique is
spray drying, due to its an ongoing process, low cost and produces
dry particles in a short time which can provide particles with high
quality [8].
The wall material which used for encapsulation must be food-
grade, biodegradable and able to form a barrier between the inter-
nal phase and its surroundings. Polysaccharides and proteins are
the most materials that are widely used for encapsulation in food
applications [3]. The present study was aimed at the development
of a combination of the gum arabic, maltodextrin, modified starch,
whey protein for microencapsulation of Fingered citron extract
(FCE) using spray drying.
2. Materials and methods
2.1. Raw materials and chemicals
Fingered citron (Citrus medica L. var. sarcodactylis Swingle) was
provided by Zhejiang Golden Hand Biological Technology Co., Ltd.
in Jinhua, Zhejiang Province, China. Gum arabic (GA) was pur-
chased from Sinopharm Chemical Reagent Co., Ltd. (SCR), China.
Maltodextrin (MD), modified starch (MS), and whey protein (WP)
were supplied by Shyuanye Co. China. All other chemicals were
analytical grade.
The mixtures were homogenized manually through stirring then
using a high-speed homogenizer (Ultra- Turrax IKA T18, IKA Works
Inc., Wilmington, NC, USA) at 10000 rpm for 2 min then 25000 rpm
for 3 min.
2.2.3. Spray drying process
Microcapsules were prepared through drying the homogenized
feed mixtures in a GEA Niro spray dryer (MOBILE MINORTM R&D
Spray Dryer, Soborg, Denmark). The mixtures fed into the drying
chamber at a feed flow rate of 17–21 mL/min. The spray dryer
operated at inlet temperatures 185 ± 2 °C and outlet temperature
80 ± 2 °C. Microcapsules powder was collected and stored in sealed
plastic bags at 5 °C [9].
2.3. Powder analysis
2.3.1. Encapsulation yield
Encapsulation yield after spray drying was calculated as a per-
centage as a ratio between the total microcapsules powders weight
and the weight of the carrier agents using Eq. (1) [10].
weight ðgÞ of the powder collected
Encapsulation Yieldð%Þ ¼
weight ðgÞ of the carrier agents
 100
ð1Þ
2.3.2. Encapsulation efficiency
Encapsulation efficiency was calculated as a percentage as a
ratio between the encapsulated and total phenolics content in
microcapsules powders using Eq. (2). Total and surface phenolic
content of microcapsules powders were determined according to
Yinbin et al. [11].

2.2. Methods Encapsulation efficiencyð%Þ

 
Phenolics content on microcapsule surface
¼ 1  100
2.2.1. Preparation of extraction Total phenolics content of microcapsule
Fingered citron extract was prepared according to the opti- ð2Þ
mized ultrasonic/microwave-assisted extraction (UMAE) process-
ing and based on previous study [2]. Fingered citron powder was
extracted with distilled water at solid/solvent ratio (1:37 g/mL), 2.3.3. Moisture content
microwave power (305.28 W), and sonication time (96.13 s). Moisture content of the microcapsules powders was deter-
Extraction temperature did not exceed 70 °C during extraction mined using air oven method [12]. The moisture content was
time, after extraction process, the Fingered citron extract was calculated as the weight loss after drying sample in a drying oven
allowed to cool to room temperature then centrifuged at at 105 °C until constant weight was obtained, as demonstrated in
4,000 rpm for 20 min. The supernatant solution was filtered under Eq. (3):
vacuum through the No.1 Whatman filter paper using a Buchner
funnel, then stored at 4 °C until use. Moisture contentð%Þ
Wet sample weight ðgÞ  Dry sample weight ðgÞ
¼  100
2.2.2. Preparation the feed mixture Wet sample weightðgÞ
The Fingered citron extract was combined with four different ð3Þ
carrier agents, abbreviated as GA, MD, MS, and WP. The carrier
agents were mixed at different rates to obtain five formulations
as shown in (Table 1). 2.3.4. Water activity (aw)
Encapsulation feed mixtures were prepared mixing the carrier Water activity of the microcapsules powders was measured
agents formulations into Fingered citron extract (10 g/100 mL). using an electronic water activity meter (Labmaster-aw, Novasina

Table 1
Design of formulations of the encapsulation carrier agents.

No. Formulation Gum arabic (%) Maltodextrin (%) Modified starch (%) Whey protein (%)
1 GMSW 25 25 25 25
2 GMS 33.33 33.33 33.33 0
3 GMW 33.33 33.33 0 33.33
4 GSW 33.33 0 33.33 33.33
5 MSW 0 33.33 33.33 33.33
 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134
AG, Neuheimstrasse, Switzeland) after microcapsules powders
samples stabilization at 25 °C for 15 min [13].
2.3.5. Hygroscopicity
Hygroscopicity of the microcapsules powders was determined
according to Rezende et al. [14]. One g of the sample was placed
with a sodium chloride saturated solution (75.29% relative humid-
ity) at 25 °C in a desiccator. After 7 days, hygroscopicity of the
microcapsules powders was calculated based on Eq. (4):
Adsorbed moisture ðgÞ
Hygroscopicityð%Þ ¼  100
Sample weight ðgÞ
2.3.6. Bulk density
Bulk density of the microcapsules powders was determined
according to Saifullah et al. [15]. Two g of samples was poured into
a 10 mL graduated measuring glass cylinder, then bulk density was
calculated as shown in Eq. (5):
Sample weight ðgÞ
Bulk density ðg cm3 Þ ¼
Sample volume ðcm3 Þ
2.3.7. Tapped density
Tapped density of the microcapsules powders was determined
according to Saifullah et al. [15]. For measuring tapped volume of
the samples, 2 g of each sample was placed in a 10 mL graduated
measuring glass cylinder and drop the cylinder gently 100 times
onto a rubber mat from a height of 20 cm. Afterward, the tapped
density was calculated according to Eq. (6):
Sample weight ðgÞ
Tapped density ðg cm3 Þ ¼
Tapped volume ðcm3 Þ
2.3.8. Particle density
Particle density of microcapsules powders was measured
according to Santhalakshmy et al. [13]. One g of dried powder sam-
ple was transferred into a 10 mL measuring cylinder with a glass
stopper. A 5 mL of petroleum ether was added to the sample and
was shaken for 30 s. then, the wall of the cylinder was washed with
2 mL of petroleum ether and the total volume were read. The par-
ticle density was calculated according to Eq. (7):
Particle density ðg cm3 Þ
Sample weight ðgÞ
¼
Total volume of petroleum ether and suspended particles ðcm3 Þ  7
2.3.9. Flowability
Flowability of the Fingered citron extract microcapsule powders
was estimated based on Carr’s index and Hausner ratio [15].
The Carr’s index (CI) was used to expresses the flow ability of
microcapsules powders based on tapped density and bulk density
[13]. The Carr’s index of the microcapsules powders was calculated
using Eq. (8):
Tapped density  Bulk density
CIð%Þ ¼  100
Tapped density
Cohesiveness of the microcapsules powders was estimated
using Hausner ratio (HR) based on tapped density and bulk density
[15]. The Hausner ratio of the microcapsules powders was calcu-
lated using Eq. (9):
Tapped density
HR ¼
Bulk density
1127
2.3.10. Porosity
Porosity of microcapsules powders measured based on particle
density and tapped density [13], and calculated by Eq. (10):
Particle density  Tapped density
Porosity ¼  100 ð10Þ
Particle density
2.3.11. Wettability
Wettability of the microcapsules powders was evaluated based
on estimating of the time (min) required to immerse 1 g of micro-
ð4Þ capsules powder on a surface of 400 mL distilled water at 25 °C
[16].
2.3.12. Solubility
Solubility of microcapsules powders was determined according
to Santhalakshmy et al. [13]. One g of microcapsules powder was
mixed and transferred into 100 mL of distilled water, stirred using
a magnetic stirrer (500 rpm for 30 min) at 25 °C, then centrifuged
at 3000 rpm for 5 min. An aliquot of 25 mL of the supernatant was
ð5Þ dried at 105 °C. Solubility of the microcapsules powders then was
calculated using Eq. (11):
Weight of the powder ðgÞ in the supernatant
Solubilityð%Þ ¼
Weight of the powder ðgÞ in the solution
 100
ð11Þ
2.3.13. Color
Color of microcapsules powders was measured using a col-
orimeter (HunterLab UltraScan PRO Spectrophotometer, Hunter
ð6Þ
Associates Laboratory, Inc., Virginia, USA). The instrument was cal-
ibrated to standard white and black tiles before measurement.
Approximately 5 g of microcapsules powder was placed in a
transparent plastic bag, the color parameters [L* (light\dark), a*
(red\green) and b* (yellow\blue)] were determined in randomly
three different surfaces of each sample [17].
2.3.14. Particle size analysis
Particle size of microcapsule powder was determined by using a
laser particle size analyzer (Microtrac S3500, Microtrac Inc., North
Largo, FL, USA). Reconstituted microcapsule was prepared through
dispersing 1 g of microcapsules powder in 100 mL of distilled
water using a magnetic stirrer (500 rpm for 30 min) at 25 °C. The
reconstituted microcapsule solution was diluted in the sample
ð7Þ chamber with deionized water. Particle size of the microcapsule
powder was expressed in micrometers (lm) [18].
2.3.15. Thermal analysis
Thermal behavior of the microcapsule powder was determined
by using a differential scanning calorimetry (DSC) (DSC Q2000, TA
Instruments, New Castle, DE, USA) according to Hu et al. [19] with
some modifications. Approximately 5 mg of the microcapsule pow-
der was heated on an aluminum pan from 25 to 250 °C at a rate of
10 °C/min under the protection of nitrogen atmosphere (50 mL/
min).
ð8Þ
2.3.16. Crystallinity (X-ray diffraction)
Crystallinity of the microcapsule powder was evaluated using
an X-ray diffractometer (D2 PHASER, Bruker AXS Co. Ltd., Karl-
sruhe, Germany) [20]. The scanning region of the diffraction angle
(2h) ranged from 5° to 80°. X-ray diffraction patterns of samples
were analyzed using software (MDI Jade 6) and calculated as rela-
ð9Þ
tive crystallinity (%) according to equation (12):
1128 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134

Relative crystallinityð%Þ
Sum of total crystalline peak areas
¼  100
Sum of total crystalline and amorphous peak areas
ð12Þ

2.3.17. Scanning electron microscopy

Particle morphology of the microcapsule powder was analyzed
using scanning electron microscopy method (SU 1510, Hitachi
Corp., Tokyo, Japan) [21]. The microcapsule powder was mounted
on a specimen holder using double scotch tape and coated with a
thin layer of gold under vacuum. Finally, the sputtered coated sam-
ples were scanned with an accelerating beam voltage of 10 kV.

2.3.18. Fourier transform infrared spectroscopy (FT-IR)

Chemical structure of the microcapsule powder was identified
using FT-IR spectrophotometer (Nicolet iS10, Thermo Fisher Scien-
tific Co. Ltd., Waltham, Massachusetts, USA) according to the estab-
lished method by Hu et al. [19]. The microcapsule powder was
blended with KBr powder in a ceramic mortar and pressed into pel-
lets then FT-IR spectrum of the samples was measured at a resolu-
tion of 4 cm1 in transmission mode from 500 to 4000 cm1
wavenumber range.

2.4. Statistical analysis

Statistical analyses were carried out using IBM SPSS 20 software

(SPSS Inc., Chicago, USA). Analysis of variance (ANOVA) was per- Fig. 1. Encapsulation yield (a), encapsulation efficiency (b) of the Fingered citron
formed in order to determine the significant differences between extract microcapsule powders. Different letters in the columns indicate significant
the samples with Duncan’s multiple range test on a 95% confidence differences (p  0.05) between the data.

level (p  0.05). All tests were carried out in triplicate, and the
mean ± standard deviation was reported.
mulations negatively affects their encapsulation efficiency. Similar
results were obtained in other studies about microcapsules loaded
3. Results and discussion with phenolic compounds (e.g., 76.56–86.74%) [11].

3.1. Encapsulation yield

3.3. Moisture content
Formulation of extract of the bioactive compounds with differ-
ent encapsulating agents to obtain microcapsule powder is of con- Moisture content is an important microcapsule characteristic
siderable importance for food [10]. Encapsulation yield in this and is correlated with water activity, flowability, stickiness, drying
research study ranged from 77.77 to 89.39%. Such yield was con- efficiency, oxidation of bioactive agents and microbial growth. Fur-
siderably satisfactory according to the criterion already reported thermore, high moisture content of microcapsule affects stability
by Du et al. [22]. Encapsulation yield of the various carrier formu- at the storage where it cause changes in wall materials from the
lation used in this research study are shown in Fig. 1.a. Encapsula- glassy state to an amorphous rubbery state. That leads to degrada-
tion yield of the GMS formulation was found the highest (89.39%). tion and releases the core material [12]. GSW formulation had the
Encapsulation yields of the formulations GMW and GSW were sig- highest moisture content followed by GMS formulation, and no
nificantly lower (p  0.05) than that of the GMS, however no signif- significant differences (p  0.05) among those of GMSW, GMW,
icant difference was found between mean values of encapsulation and MSW formulations were found (Table 2). Moisture content of
yield of GMW and GSW. Encapsulation yield of MSW was the low- Fingered citron extract microcapsule powders is generally less
est (77.77%), but its mean value was not significantly different than 6%, hence it meets the moisture content requirement of a food
(p  0.05) from that of the GMSW. Because gum arabic is known powder (4–6%) [24] and it is suitable for long-term storage [25].
to have high capability of film forming, microcapsules that have
high percentage of gum arabic were found to be of high encapsula-
tion yield. Hence encapsulation yield of MSW was found to be the
Table 2
lowest among all microcapsules used in this research study.
Moisture, water activity, and hygroscopicity of the Fingered citron extract microcap-
sule powders.
3.2. Encapsulation efficiency
Parameters Moisture (%) Water activity Hygroscopicity (%)
GMSW 4.50 ± 0.461a 0.229 ± 0.005a 10.26 ± 0.46c
Efficiency is an important parameter in the improvement of an
GMS 5.63 ± 0.415b 0.299 ± 0.006b 9.50 ± 0.35ab
encapsulation procedure, regardless of the processes and the mate- GMW 4.67 ± 0.220a 0.333 ± 0.011c 9.27 ± 0.22ab
rials encapsulated [23]. Encapsulation efficiency for each type of GSW 5.70 ± 0.405b 0.312 ± 0.008b 9.68 ± 0.24b
carrier agent formulations was evaluated based on the amount of MSW 4.78 ± 0.314a 0.303 ± 0.005b 9.04 ± 0.27a
the encapsulated phenolics. Encapsulation efficiency values as The results are expressed as the mean value ± standard deviation (n = 3). Different
shown in Fig. 1b, ranged from 72.11 to 87.20%. It is apparent that letters in the same column indicate significant differences (p  0.05) between the
the presence of whey protein and absence the gum arabic in for- data.
 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134 1129

3.4. Water activity (aw)
Table 2 shows water activity mean values of the Fingered citron
extract microcapsule powders. GMW formulation had the highest
water activity, whilst GMSW formulation had the lowest water
activity and no significant differences (p  0.05) among moisture
content mean values of GMS, GSW, and MSW formulations. As it
is depicted within Table 2, water activity of Fingered citron extract
microcapsule powders ranged from 0.23 to 0.33. Such values indi-
cates that Fingered citron extract microcapsule powders are con-
sidered stable materials concerning microbial contamination
where water activity values were lower than 0.6. Low water activ-
ity would limit microbial growth, overcome caking problems,
improve physicochemical stability and total acceptability [25].
3.5. Hygroscopicity
Hygroscopicity is the ability of a material to absorb moisture
from the atmosphere. Hygroscopicity, when it is high would cause
aggregation of the spray dried powder, which affects the nutri-
tional and flow properties of the powder. Hygroscopicity of GMSW
formulation was significantly high (p  0.05) compared to those of
the other formulations. The lowest hygroscopicity mean value was
that of MSW formulation (Table 2). Hygroscopicity mean values of
the Fingered citron extract microcapsule powders of this research
study was lower than hygroscopicity values that were reported
in previous studies using gum arabic as wall material, including
Gagaita fruit extract (14.8–18.8%) [26]. Similar results were
reported for microencapsulated refined kenaf seed oil (7.8–10.1%)
[25].
3.6. Bulk density
Bulk density mean values of the formulations of this research
study, as shown in table 3, ranged from 0.28 to 0.44 g cm3. Similar
range of bulk density for the microencapsulated powders prepared
using spray drying (0.28–0.40 g cm3) have been reported [27].
Bulk density of the GMS formulation was significantly high
(p  0.05) compared to those of the other formulations, while no
significant differences (p  0.05) among mean values of GMSW,
GMW, GSW, and MSW formulations. Higher bulk density indicates
a lower amount of air presented in the powder, which can help to
prevent lipid oxidation during storage [25].
powders, as shown within Table 3, ranged from 0.47 to
0.60 g cm3. GMS formulation displays the highest tapped density,
followed by MSW formulation. GMW formulation had the lowest
tapped density and no significant differences (p  0.05) between
mean values of GMSW, and GSW formulations. Tapped density
mean values of Fingered citron extract microcapsule powders in
this study were close to those of the tapped density values already
reported [25].
3.8. Particle density
Particle density of Fingered citron extract microcapsule pow-
ders, as shown within table 3, varied from 1.43 to 1.83 g cm3. Par-
ticle density mean value of MSW formulation was significantly
lower (p  0.05) compared to those of the other formulations,
while that of GMS formulation was found to be the highest. Particle
density mean values of Fingered citron extract microcapsule pow-
ders of this research study were found to be higher than (0.7–
1.2 g cm3) for microencapsulated refined kenaf seed oil [25].
3.9. Flowability
Carr’s index and Hausner ratio are two closely related empiri-
cally derived parameters that allow assessing flow behavior based
on bulk and tapped densities [28]. Results of this research study
showed that Carr’s index mean values were in the range of
27.35–43.59%, indicating poor powder flowability. Hausner ratio
mean values were in the range of 1.38–1.87%, indicating high pow-
der cohesiveness. As it is shown in Table 4, mean values of CI and
HR for all formulations were high and significantly different
(p  0.05) from each other. GMSW, GSW, and MSW formulations
were of awful flowing powders. GMW formulation was of very
poor flowing, while GMS formulation was of poor flowing. Powders
of all formulations were found of poor flow behaviors, but the pow-
ders were easily compressible. High mean values of CI and HR indi-
cate poor flowability and they are generally related to high values
of the interparticle friction [29]. Microcapsule powders that are
obtained in this research study were very compressible. Similar
mean values of CI (33.72–48.65%) and HR (1.53–1.96) for microen-
capsulation of flax oil with zein [30].
3.10. Porosity

3.7. Tapped density
Tapped density of powders is a variable that affects the packag-
ing, transportation, and commercialization of powders and indi-
cates the weight of powder that can fit in a container. The
advantage of produce spray dried powders with higher tapped
density is the smaller containers required to store [27]. Tapped
density mean values of Fingered citron extract microcapsule
Porosity is an important property in the food industry especially
in the reconstitution of dry powders. The porosity of the powders
indicates the ratio of the volume of voids between the particles
and the volume of pores to the total volume occupied by the pow-
der [25].
Porosity mean values of Fingered citron extract microcapsule
powders formulations of this research study ranged from 61.37
to 74.45%. Significant differences (p  0.05) among mean values
of all formulations were found (Table 5). Mean value of GMW for-

Table 3
Bulk density, tapped density, and particle density of the Fingered citron extract Table 4
microcapsule powders. Carr’s index, Hausner ratio, flowability and of the Fingered citron extract microcap-
sule powders.
Parameters Bulk density Tapped density Particle density
(g cm3) (g cm3) (g cm3) Parameters Carr’s index (%) Hausner ratio Flowability
GMSW 0.30 ± 0.014b 0.55 ± 0.03b 1.67 ± 0.09a GMSW 45.13 ± 0.80d 1.82 ± 0.03d Awful
GMS 0.44 ± 0.02a 0.60 ± 0.03a 1.83 ± 0.096a GMS 27.35 ± 0.10a 1.38 ± 0.00a Poor
GMW 0.29 ± 0.02b 0.47 ± 0.02c 1.67 ± 0.09a GMW 37.21 ± 0.05b 1.59 ± 0.00b Very poor
GSW 0.28 ± 0.01b 0.53 ± 0.03b 1.67 ± 0.09a GSW 46.59 ± 0.36f 1.87 ± 0.01f Awful
MSW 0.31 ± 0.02b 0.55 ± 0.02ab 1.43 ± 0.08b MSW 43.96 ± 0.62c 1.78 ± 0.02c Awful

The results are expressed as the mean value ± standard deviation (n = 3). Different The results are expressed as the mean value ± standard deviation (n = 3). Different
letters in the same column indicate significant differences (p  0.05) between the letters in the same column indicate significant differences (p  0.05) between the
data. data.
1130 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134

Table 5 Table 6
Porosity, wettability, and solubility of the Fingered citron extract microcapsule Color parameters of the Fingered citron extract microcapsule powders.
powders.
Parameters L* a* b*
Parameters Porosity (%) Wettability (min) Solubility (%)
GMSW 94.90 ± 4.75a 0.79 ± 0.03c 8.66 ± 0.52b
GMSW 67.33 ± 0.30c 14.44 ± 0.92c 79.44 ± 4.88b GMS 95.61 ± 5.74a 0.53 ± 0.03a 7.14 ± 0.29a
GMS 61.38 ± 0.45a 11.88 ± 0.91a 70.62 ± 3.37c GMW 95.27 ± 3.81a 0.73 ± 0.04bc 8.16 ± 0.41b
GMW 74.45 ± 0.04f 13.08 ± 0.82abc 91.26 ± 4.26a GSW 94.62 ± 5.68a 0.71 ± 0.03b 9.01 ± 0.45b
GSW 68.50 ± 0.08d 12.76 ± 0.80ab 70.09 ± 2.38c MSW 94.64 ± 3.79a 0.74 ± 0.04bc 8.64 ± 0.52b
MSW 63.86 ± 0.08b 13.83 ± 0.76bc 71.67 ± 2.33c
L* (luminosity degree), a* (degree of redness to greenness), b* (degree of yellowness
The results are expressed as the mean value ± standard deviation (n = 3). Different to blueness).The results are expressed as the mean value ± standard deviation
letters in the same column indicate significant differences (p  0.05) between the (n = 3). Different letters in the same column indicate significant differences
data. (p  0.05) between the data.

mulation was the highest, while that of GMS formulation was the
lowest. Mean values of porosity in all formulations in this research
study were found to be in agreement with results [31] where the
porosity mean values ranged from 68 to 75%. High values of poros-
ity indicate presence of a considerable number of spaces between
particles, which hold oxygen that may cause degradation reactions
[13].
3.11. Wettability
Wettability of microcapsules indicates its ability to absorb
water that related to the reconstitution of the powder. The shorter
time for the powder to dissolute into water, the better its physical
attribute in food processing [25]. Wettability mean values of
microcapsule powders varied from 11.88 to 14.44 min. Wettability
mean values of all formulations carried out in this research study
are tabulated in Table 5. Wettability mean value of GMSW formu-
lation was the highest, but not significantly different (p  0.05)
from those of GMW and MSW. Wettability mean value of GMS for-
mulation was the lowest, but not significantly different (p  0.05)
from those of GMW and GSW all other means of formulations in
this research study. No significant differences (p  0.05) were
found among wettability mean values of GMS, GMW and GSW for-
mulations. Range of wettability (11.88–14.44 min) for the micro-
capsule powders obtained in this research was wider than the
range (6–10 min) already reported [25] for refined kenaf seed oil
microcapsule powders.
3.12. Solubility
Solubility is the last particle dissolution step and is a decisive
factor for quality of powder that are used as ingredients in food
industry. Poor soluble powders may cause processing difficulties
and economic losses [32]. Solubility mean values of Fingered citron
extract microcapsule powders, as listed in Table 5, ranged from
70.09 to 91.26%. Solubility mean value of the GMW formulation
was significantly high (p  0.05) compared to those of other formu-
lations. No significant differences (p  0.05) among solubility mean
values of GMS, GSW, MSW formulations were found. Solubility
result of Fingered citron extract microcapsule powders obtained
in this research study is considerably higher than the solubility
of spray dried persimmon powders (52.96–76.22%) [22].
Lightness mean values (L*) ranged from 94.62 to 95.61, which indi-
cates that all samples tend to be of white color. Mean values of (a*)
ranged from 0.53 to 0.79, which indicates that all samples tend
to be of green color. GMS formulation had an (a*) mean value that
was found significantly lower (p  0.05) compared to mean values
of other formulations. Mean values of (b*) ranged from 7.14 to 9.01
which indicates that all samples tend to be of yellow color. GMS
formulation had a (b*) mean value that was found significantly
lower (p  0.05) compared to mean values of other formulations
and this might be attributed to its high whey protein content.
3.14. Particle size analysis
Because it affects quality and flowability of final product, parti-
cle size is taken into consideration during powder processing for-
mulation. [29]. Appearance, dispensability, and flowability of
microcapsule powders are highly influenced by particle size [32].
Mean values of particle size diameter of Fingered citron extract
microcapsule powders as depicted in Fig. 2 ranged from 14.34 to
26.47 lm. MSW formulation had the highest particle size, whilst
GMW formulation had the lowest particle size and no significant
differences (p  0.05) among particle size of GMSW, GMS, and
GSW formulations were found. Particles size of Fingered citron
extract microcapsule powders formulated in this research study
met particle size requirement of a microcapsules food powder
(10–100 mm) according to Fang and Bhandari [33]. Distribution
of particle size for reconstituted microcapsule formulations exhib-
ited different distribution peaks in a range of 0.26–87.99 lm
(Fig. 3). GMSW and GMW formulations showed a heterogeneous
size were they exhibited distribution with two different peaks. Par-
ticle size values of microcapsule powders formulated in this study
are consistent with results reported by Fernandes et al. [32].

3.13. Color

Color parameters, including luminosity L* (the degree of light-

ness on 0–100 scale from black to white), a* [the degree of redness
(+) to greenness ()], and b* [the degree of yellowness (+) to blue-
ness ()] are shown in Table 6 [11].
As it can be seen from Table 6, no significant differences Fig. 2. Mean particle size of the Fingered citron extract microcapsule powders.
(p  0.05) were found among lightness (L*) mean values of micro- Different letters in the columns indicate significant differences (p  0.05) between
capsule powders formulations obtained in this research study. the data.
 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134
Fig. 3. Particle size distribution curves of rehydrated of the Fingered citron extract
microcapsule powders.
3.15. Thermal analysis
Thermal behavior of Fingered citron extract microcapsule pow-
ders evaluated by DSC is presented in Fig. 4. The formulations
showed endothermic peaks ranged between 155.85 and 189.47 °C.
Optimal thermal stability of Fingered citron extract microcap-
sule powders was achieved when GMW formulation was used as
wall materials. GMW formulation was significantly high
(p  0.05). Results showed that presence of modified starch in for-
mulations negatively affects thermal stability. In presence of mal-
todextrin however, starch has a positive effect, but whey protein
has better effect compared with maltodextrin. Formulations that
contain gum arabic, whey protein and maltodextrin were found
of superior thermal stability.
Thermal stability findings in this research study were consistent
with the results obtained by Kang et al. [12] who investigated ther-
mal behavior of chlorophylls microcapsules by gum aribic and mal-
todextrin in different ratios. They indicated that thermal stability
was improved using gum aribic and maltodextrin as wall materi-
als, and optimal thermal stability was obtained when maltodextrin
was used as wall material. Similar thermal behavior of grape skin
extract has been obtained by Kalušević et al. [34].
Fig. 4. Thermal stability of the Fingered Citron extract microcapsule powders.
Different letters in the columns indicate significant differences (p  0.05) between
the data.
1131
3.16. Crystallinity (X-ray diffraction)
Because crystallinity of microcapsules is related to their stabil-
ity, it is important to determine whether the microcapsules have
crystalline or amorphous structures through XRD analysis. The X-
ray diffraction patterns of the Fingered citron extract microcapsule
powders was presented in Fig. 5. Relative crystallinity of Fingered
citron extract microcapsule powders ranged between 18.20 and
46.13%, where GMW formulation showed to be of the smallest rel-
ative crystallinity compared with other formulations, while GMS
formulation was of the highest relative crystallinity.
Formulation with no modified starch showed a small tendency
for crystallization. Because of its higher relative crystallinity com-
pared to the other formulation, GMS formulation may have high
storage stability. Amorphous samples tend to be very hygroscopic
and would absorb water during storage. Samples then become
sticky and form agglomerates as the amorphous sugars are trans-
formed into crystalline sugars. This characteristic prejudices the
storage of the samples since water absorption implicates in weight
gain and nutrient degradation, microstructure collapse, and poten-
tial microbiological instability [35].
3.17. Scanning electron microscopy (SEM)
Microstructures of Fingered citron extract microcapsule pow-
ders are depicted through SEM micrographs shown in (Fig. 6) the
samples were examined by SEM in order to determine the presence
of fractures, cracks, or any other possible defects that could expose
since any fracture may lead to the degradation and oxidation of the
exposed encapsulated material [36].
The micrographs by SEM showed the shape of the microcap-
sules which appeared spherical, and semi-spherical, though the
typical shape of spray dried particles should be spherical, with a
mean size of 10–100 mm [33]. The SEM micrograph also showed
dents, rough, wrinkled surfaces and slight agglomeration. Frac-
tured microcapsules were observed in powders of GMSW and
MSW formulations, which might be attributed to the low drying
temperature as well as viscoelastic and film-forming properties.
It is apparent that microcapsules had various sizes and that
might be related to an increase in inlet temperature in the spray
dryer, as it accelerated the rate of drying of the droplets. It is noted
that there was some cracks, breaks, and contractions in microcap-
Fig. 5. Relative crystallinity by X-ray diffraction patterns of the Fingered citron
extract microcapsule powders.
1132 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134
Fig. 6. Scanning electronic microscopy of the Fingered citron extract microcapsule
powders, (a) GMSW formulation; (b) GMS formulation; (c) GMW formulation; (d)
GSW formulation; (f) MSW formulation.
sules, where that might be attributed to the high rate of steam gen-
eration and the rapidly crust expanded [10]. Results of SEM analy-
sis in this research study were in agreement with those presented
in previous studies that showed irregular spherical shaped parti-
cles with many shrinkages and dents on the surface [25–27,32].
Different morphologies and irregular surfaces might be related
to differences in feeding ratio, droplet size, and temperature
through drying process. Shrinkage of the particle followed by an
incipient expansion may induce changes in the size of particles
and broken shells. Moreover, the irregularity on the surface of
the microcapsules may be desirable in terms of its enhanced dis-
persibility and the rehydration of the powders [36].
3.18. Fourier transform infrared spectroscopy (FT-IR)
FT-IR spectra of the raw materials (GA, MD, MS, and WP), the
microcapsules (GMSW, GMS, GMW, and GSW) and Fingered citron
extract are shown in Fig. 7.
Absorption bands in the spectrum of gum arabic were observed
at 3276 cm1 (OAH stretching), 2919 cm1 (CAH stretching from
the carboxylic group), 1602 cm1 (C@O stretching or NAH bend-
ing), 1415 cm1 (CH3 bending and CAH bending), and 1022 cm1
(CAO stretching) and this result was similar to Chew et al. [25].
Maltodextrin spectrum showed absorption bands at 3291 cm1
(OAH stretching), 2920 cm1 (CAH stretching from the carboxylic
group), 1644 cm1 (C@O stretching), 1360 cm1 (OAH bending),
and 1150 cm1, 1078 cm1, 1001 cm1 (CAO stretching and
CAOAH bending) and this was in agreement with Kang et al. [12].
Fig. 7. FT-IR spectra of gum arabic (GA), maltodextrin (MD), modified starch (MS),
whey protein (WP), Fingered citron extract microcapsule powders (GMSW, GMS,
GMW, GSW, and MSW) and Fingered citron extract (FCE).
Absorption bands of modified starch, as shown within the FT-IR
spectra, were observed at 3275 cm1 (OAH stretching), 2938 cm1
(CAH stretching from the carboxylic group), 1641 cm1 (C@O
stretching), 1335 cm1 (CH3 bending), 1145 cm1, 1074 cm1,
and 993 cm1 (CAO stretching and CAOAH bending). Similar
results were obtained in previous studies [25,37].
Absorption bands of whey protein were observed at 3280 cm1
(OAH stretching), 2927 cm1 (CAH stretching from the carboxylic
group), 1630 cm1 (Amide I, C@O stretching), 1520 cm1,
1446 cm1, 1390 cm1 (Amide type II, N-H bending) and
1064 cm1 (CAO stretching and C-O-H bending). These results
are in agreement with Hu et al. [19] and Hosseinnia et al. [37].
For the microcapsules, characteristic hydroxyl peaks (OAH
stretching) were observed around 3280 cm1. Peaks corresponding
to the CAH stretching from the carboxylic group appeared around
2920 cm1. Peaks corresponding to amine or carbonyl group
appeared at 1601 cm1 in the GMS formulation around
1635 cm1 in other formulations. Amide ΙΙ (1530 cm1) appeared
in all formulations except GMS formulation, and that might be
attributed to absence of whey protein. Peaks 1150 cm1,
1075 cm1, and 1020 cm1 which corresponding to C-O stretching
and C-O-H bending appeared in all formulations [12,19,25,37].
Fingered citron extract spectrum showed an absorption band at
2935 cm1 which attributed to the asymmetric C-H stretching of
the methyl groups that are present in most of the phenolic com-
pounds [37]. It is noticeable that the bands (1973, 2031 and
2165 cm1) appeared in all microcapsules but did not appear in
Fingered citron extract spectra. In addition, the Amide ΙΙ band
(1530 cm1) has not appeared in Fingered citron extract spectra
but it appeared in all formulations that contain whey protein.
The spectra of microcapsules and Fingered citron extract confirmed
that the microencapsulation by spray drying was successfully
achieved, where there was no core material on the surfaces of
the microcapsules.
4. Conclusions
The microcapsules produced by using gum arabic/maltodex-
trin/modified starch (GMS) was chosen as an optimum encapsula-
tion process due to its superiority in most of the properties, where
it provided the highest encapsulation yield and efficiency. More-
 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134
over, GMS microcapsules showed the highest bulk, tapped, and
particle density, which indicated a good storage stability. On the
other hand, GMS microcapsules had the lowest porosity and
shorter time for wettability, which inferred a good ability to recon-
stitute the powders. Furthermore, the X-ray diffraction showed
that the GMS microcapsules had the highest relative crystallinity,
which demonstrated the highest storage stability among other for-
mulations. In addition, the GMS microcapsules beside two other
formulations showed spherical and semi-spherical without crack-
ing. FT-IR analysis showed no appearance of core material on the
surfaces of the microcapsules in all formulations.
Further study will be conceded to investigate the antioxidant
properties of the Fingered citron extract microcapsules powders,
beside the preparation of effervescent tablets from the microcap-
sules powders in order to provide them in a manner suitable for
consumption.
Acknowledgement
This work was supported by National first-class discipline pro-
gram of Food Science and Technology (JUFSTR20180204), and
China Scholarship Council (CSC) Beijing, China (CSC
No.2015886031). This work carried out in the Laboratory of the
National Engineering Research Center for Functional Food at Jiang-
nan University, Wuxi, China.
References
[1] Z. Wu, H. Li, Y. Yang, Y. Zhan, D. Tu, Variation in the components and
antioxidant activity of Citrus medica L. var. sarcodactylis essential oils at
different stages of maturity, Ind. Crops Prod. 46 (2013) 311–316, https://doi.
org/10.1016/j.indcrop.2013.02.015.
[2] A.A. Mahdi, M.M.A. Rashed, W. Al-Ansi, M.I. Ahmed, M. Obadi, Q. Jiang, H. Raza,
H. Wang, Enhancing bio-recovery of bioactive compounds extracted from
Citrus medica L. Var. sarcodactylis: optimization performance of integrated of
pulsed-ultrasonic/microwave technique, J. Food Meas. Charact. 1661–1673
(2019), https://doi.org/10.1007/s11694-019-00083-x.
[3] V. Nedovic, A. Kalusevic, V. Manojlovic, S. Levic, B. Bugarski, An overview of
encapsulation technologies for food applications, Proc. Food Sci. 1 (2011)
1806–1815, https://doi.org/10.1016/j.profoo.2011.09.265.
[4] L. de Souza Simões, D.A. Madalena, A.C. Pinheiro, J.A. Teixeira, A.A. Vicente, O.L.
Ramos, Micro-and nano bio-based delivery systems for food applications:
in vitro behavior, Adv. Colloid Interface Sci. 243 (2017) 23–45, https://doi.org/
10.1016/j.cis.2017.02.010.
[5] S. Ray, U. Raychaudhuri, R. Chakraborty, An overview of encapsulation of active
compounds used in food products by drying technology, Food Biosci. 13 (2016)
76–83, https://doi.org/10.1016/j.fbio.2015.12.009.
[6] M.A. Augustin, Y. Hemar, Nano-and micro-structured assemblies for
encapsulation of food ingredients, Chem. Soc. Rev. 38 (4) (2009) 902–912,
https://doi.org/10.1039/B801739P.
[7] A.B. Das, V. Goud, C. Das, Microencapsulation of anthocyanin extract from
purple rice bran using modified rice starch and its effect on rice dough
rheology, Int. J. Biol. Macromol. 124 (2019) 573–581, https://doi.org/10.1016/j.
ijbiomac.2018.11.247.
[8] A.S. Mahdavi, S.M. Jafari, E. Assadpour, M. Ghorbani, Storage stability of
encapsulated barberry’s anthocyanin and its application in jelly formulation, J.
Food Eng. 181 (2016) 59–66, https://doi.org/10.1016/j.jfoodeng.2016.03.003.
[9] S.A. Korma, W. Wei, A.H. Ali, S.M. Abed, L. Zheng, Q. Jin, X. Wang, Spray-dried
novel structured lipids enriched with medium-and long-chain triacylglycerols
encapsulated with different wall materials: characterization and stability,
Food Res. Int. 116 (2019) 538–547, https://doi.org/10.1016/
j.foodres.2018.08.071.
[10] M.V. Álvarez-Henao, N. Saavedra, S. Medina, C.J. Cartagena, L.M. Alzate, J.
Londoño-Londoño, Microencapsulation of lutein by spray-drying:
characterization and stability analyses to promote its use as a functional
ingredient, Food Chem. 256 (2018) 181–187, https://doi.org/10.1016/
j.foodchem.2018.02.059.
[11] L. Yinbin, L. Wu, M. Weng, B. Tang, P. Lai, J. Chen, Effect of different
encapsulating agent combinations on physicochemical properties and stability
of microcapsules loaded with phenolics of plum (Prunus salicina lindl.),
Powder Technol. 340 (2018) 459–464, https://doi.org/10.1016/j.
powtec.2018.09.049.
[12] Y.-R. Kang, Y.-K. Lee, Y.J. Kim, Y.H. Chang, Characterization and storage
stability of chlorophylls microencapsulated in different combination of gum
Arabic and maltodextrin, Food Chem. 272 (2019) 337–346, https://doi.org/
10.1016/j.foodchem.2018.08.063.
1133
[13] S. Santhalakshmy, S.J.D. Bosco, S. Francis, M. Sabeena, Effect of inlet
temperature on physicochemical properties of spray-dried jamun fruit juice
powder, Powder Technol. 274 (2015) 37–43, https://doi.org/10.1016/j.
powtec.2015.01.016.
[14] Y.R.R.S. Rezende, J.P. Nogueira, N. Narain, Microencapsulation of extracts of
bioactive compounds obtained from acerola (Malpighia emarginata DC) pulp
and residue by spray and freeze drying: chemical, morphological and
chemometric characterization, Food Chem. 254 (2018) 281–291, https://doi.
org/10.1016/j.foodchem.2018.02.026.
[15] M. Saifullah, Y. Yusof, N. Chin, M. Aziz, Physicochemical and flow properties of
fruit powder and their effect on the dissolution of fast dissolving fruit powder
tablets, Powder Technol. 301 (2016) 396–404, https://doi.org/10.1016/j.
powtec.2016.06.035.
[16] F.Z. Vissotto, L.C. Jorge, G.T. Makita, M.I. Rodrigues, F.C. Menegalli, Influence of
the process parameters and sugar granulometry on cocoa beverage powder
steam agglomeration, J. Food Eng. 97 (3) (2010) 283–291, https://doi.org/
10.1016/j.jfoodeng.2009.10.013.
[17] W. AL-Ansi, A.A. Mahdi, Q.A. Al-Maqtari, M. Fan, L. Wang, Y. Li, H. Qian, H.
Zhang, Evaluating the role of microwave-baking and fennel (Foeniculum
vulgare L.)/nigella (Nigella sativa L.) on acrylamide growth and antioxidants
potential in biscuits, J. Food Meas. Charact. (2019) 2426–2437. https://doi.org/
10.1007/s11694-019-00163-y.
[18] W. Chen, G. Liang, X. Li, Z. He, M. Zen, D. Gao, F. Qin, H.D. Goff, J. Chen, Impact
of soy proteins, hydrolysates and monoglycerides at the oil/water interface in
emulsions on interfacial properties and emulsion stability, Colloids Surf. B. 177
(2019) 550–558, https://doi.org/10.1016/j.colsurfb.2019.02.020.
[19] Y. Hu, Y. Li, W. Zhang, G. Kou, Z. Zhou, Physical stability and antioxidant
activity of citrus flavonoids in arabic gum-stabilized microcapsules:
Modulation of whey protein concentrate, Food Hydrocoll. 77 (2018) 588–
597, https://doi.org/10.1016/j.foodhyd.2017.10.037.
[20] Z. Li, L. Wang, Z. Chen, Q. Yu, W. Feng, Impact of binding interaction
characteristics on physicochemical, structural, and rheological properties of
waxy rice flour, Food Chem. 266 (2018) 551–556, https://doi.org/10.1016/
j.foodchem.2018.05.010.
[21] R. Liang, Q. Huang, J. Ma, C.F. Shoemaker, F. Zhong, Effect of relative humidity
on the store stability of spray-dried beta-carotene nanoemulsions, Food
Hydrocoll. 33 (2) (2013) 225–233, https://doi.org/10.1016/
j.foodhyd.2013.03.015.
[22] J. Du, Z.-Z. Ge, Z. Xu, B. Zou, Y. Zhang, C.-M. Li, Comparison of the efficiency of
five different drying carriers on the spray drying of persimmon pulp powders,
Dry. Technol. 32 (10) (2014) 1157–1166, https://doi.org/10.1080/
07373937.2014.886259.
[23] V.B. de Souza, M. Thomazini, M.A.E. Barrientos, C.M. Nalin, R. Ferro-Furtado, M.
I. Genovese, C.S. Favaro-Trindade, Functional properties and encapsulation of a
proanthocyanidin-rich cinnamon extract (Cinnamomum zeylanicum) by
complex coacervation using gelatin and different polysaccharides, Food
Hydrocoll. 77 (2018) 297–306, https://doi.org/10.1016/j.foodhyd.2017.09.040.
[24] G.V. Barbosa-Canovas, P. Juliano, Compression and compaction characteristics
of selected food powders, Adv. Food Nutr. Res. 49 (1) (2005) 233–300, https://
doi.org/10.1016/S1043-4526(05)49006-3.
[25] S.C. Chew, C.P. Tan, K.L. Nyam, Microencapsulation of refined kenaf (Hibiscus
cannabinus L.) seed oil by spray drying using b-cyclodextrin/gum
arabic/sodium caseinate, J. Food Eng. 237 (2018) 78–85, https://doi.org/
10.1016/j.jfoodeng.2018.05.016.
[26] L.D. Daza, A. Fujita, C.S. Fávaro-Trindade, J.N. Rodrigues-Ract, D. Granato, M.I.
Genovese, Effect of spray drying conditions on the physical properties of
Cagaita (Eugenia dysenterica DC.) fruit extracts, Food Bioprod. Process. 97
(2016) 20–29, https://doi.org/10.1016/j.fbp.2015.10.001.
[27] H.C.F. Carneiro, R.V. Tonon, C.R.F. Grosso, M.D. Hubinger, Encapsulation
efficiency and oxidative stability of flaxseed oil microencapsulated by spray
drying using different combinations of wall materials, J. Food Eng. 115 (4)
(2013) 443–451, https://doi.org/10.1016/j.jfoodeng.2012.03.033.
[28] A. Saker, M.G. Cares-Pacheco, P. Marchal, V. Falk, Powders flowability
assessment in granular compaction: What about the consistency of Hausner
ratio?, Powder Technol. 354 (2019) 52–63, https://doi.org/10.1016/j.
powtec.2019.05.032.
[29] M. Ong, Y. Yusof, M. Aziz, N. Chin, N.M. Amin, Characterisation of fast
dispersible fruit tablets made from green and ripe mango fruit powders, J.
Food Eng. 125 (2014) 17–23, https://doi.org/10.1016/j.jfoodeng.2013.10.014.
[30] S. Quispe-Condori, M.D.A. Saldaña, F. Temelli, Microencapsulation of flax oil
with zein using spray and freeze drying, LWT-Food Sci. Technol. 44 (9) (2011)
1880–1887, https://doi.org/10.1016/j.lwt.2011.01.005.
[31] R.V. Tonon, C. Brabet, M.D. Hubinger, Anthocyanin stability and antioxidant
activity of spray-dried açai (Euterpe oleracea Mart.) juice produced with
different carrier agents, Food Res. Int. 43 (3) (2010) 907–914, https://doi.org/
10.1016/j.foodres.2009.12.013.
[32] R.V.d.B. Fernandes, S.V. Borges, D.A. Botrel, Gum arabic/starch/maltodextrin/
inulin as wall materials on the microencapsulation of rosemary essential oil,
Carbohydr. Polym. 101 (2014) 524–532. https://doi.org/10.1016/
j.carbpol.2013.09.083.
[33] Z. Fang, B. Bhandari, Encapsulation of polyphenols – a review, Trends Food Sci.
Technol. 21 (10) (2010) 510–523, https://doi.org/10.1016/j.tifs.2010.08.003.
[34] A.M. Kalušević, S.M. Lević, B.R. Čalija, J.R. Milić, V.B. Pavlović, B.M. Bugarski, V.
A. Nedović, Effects of different carrier materials on physicochemical properties
of microencapsulated grape skin extract, J. Food Sci. Technol. 54 (11) (2017)
3411–3420, https://doi.org/10.1007/s13197-017-2790-6.
1134 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134

[35] D. Borrmann, A.P.T.R. Pierucci, S.G.F. Leite, M.H.M.d.R. Leão, and their microencapsulates obtained by spray-drying, J. Food Eng. 112 (1–2)
Microencapsulation of passion fruit (Passiflora) juice with n- (2012) 29–37, https://doi.org/10.1016/j.jfoodeng.2012.03.032.
octenylsuccinate-derivatised starch using spray-drying, Food Bioprod. [37] M. Hosseinnia, M.A. Khaledabad, H. Almasi, Optimization of Ziziphora
Process. 91 (1) (2013) 23–27, https://doi.org/10.1016/j.fbp.2012.08.001. clinopodiodes essential oil microencapsulation by whey protein isolate and
[36] A.Y. Guadarrama-Lezama, L. Dorantes-Alvarez, M.E. Jaramillo-Flores, C. Pérez- pectin: a comparative study, Int. J. Biol. Macromol. 101 (2017) 958–966,
Alonso, K. Niranjan, G.F. Gutiérrez-López, L. Alamilla-Beltrán, Preparation and https://doi.org/10.1016/j.ijbiomac.2017.03.190.
characterization of non-aqueous extracts from chilli (Capsicum annuum L.)