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

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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-

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

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- The mixtures were homogenized manually through stirring then
tion into dry food systems [6]. using a high-speed homogenizer (Ultra- Turrax IKA T18, IKA Works
Microencapsulation is a useful way to enhance the bioavailabil- Inc., Wilmington, NC, USA) at 10000 rpm for 2 min then 25000 rpm
ity and stability of bioactive compounds and controlling the release for 3 min.
of the active agent, the main aim of encapsulation is to protect core
material from environmental effects, thereby increases shelf life of 2.2.3. Spray drying process
product and control release of the core material [7]. Microcapsules were prepared through drying the homogenized
There are several types of encapsulation technique, such as a feed mixtures in a GEA Niro spray dryer (MOBILE MINORTM R&D
centrifugal extrusion, vibrational nozzle, co-crystallization, freeze Spray Dryer, Soborg, Denmark). The mixtures fed into the drying
drying, and spray drying. The most regularly used technique is chamber at a feed flow rate of 17–21 mL/min. The spray dryer
spray drying, due to its an ongoing process, low cost and produces operated at inlet temperatures 185 ± 2 °C and outlet temperature
dry particles in a short time which can provide particles with high 80 ± 2 °C. Microcapsules powder was collected and stored in sealed
quality [8]. plastic bags at 5 °C [9].
The wall material which used for encapsulation must be food-
grade, biodegradable and able to form a barrier between the inter-
2.3. Powder analysis
nal phase and its surroundings. Polysaccharides and proteins are
the most materials that are widely used for encapsulation in food
2.3.1. Encapsulation yield
applications [3]. The present study was aimed at the development
Encapsulation yield after spray drying was calculated as a per-
of a combination of the gum arabic, maltodextrin, modified starch,
centage as a ratio between the total microcapsules powders weight
whey protein for microencapsulation of Fingered citron extract
and the weight of the carrier agents using Eq. (1) [10].
(FCE) using spray drying.
weight ðgÞ of the powder collected
Encapsulation Yieldð%Þ ¼
2. Materials and methods weight ðgÞ of the carrier agents
 100
2.1. Raw materials and chemicals
ð1Þ
Fingered citron (Citrus medica L. var. sarcodactylis Swingle) was
provided by Zhejiang Golden Hand Biological Technology Co., Ltd. 2.3.2. Encapsulation efficiency
in Jinhua, Zhejiang Province, China. Gum arabic (GA) was pur- Encapsulation efficiency was calculated as a percentage as a
chased from Sinopharm Chemical Reagent Co., Ltd. (SCR), China. ratio between the encapsulated and total phenolics content in
Maltodextrin (MD), modified starch (MS), and whey protein (WP) microcapsules powders using Eq. (2). Total and surface phenolic
were supplied by Shyuanye Co. China. All other chemicals were content of microcapsules powders were determined according to
analytical grade. 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 1127

AG, Neuheimstrasse, Switzeland) after microcapsules powders 2.3.10. Porosity

samples stabilization at 25 °C for 15 min [13]. Porosity of microcapsules powders measured based on particle
density and tapped density [13], and calculated by Eq. (10):
2.3.5. Hygroscopicity
Particle density  Tapped density
Hygroscopicity of the microcapsules powders was determined Porosity ¼  100 ð10Þ
Particle density
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 2.3.11. Wettability
microcapsules powders was calculated based on Eq. (4): Wettability of the microcapsules powders was evaluated based
on estimating of the time (min) required to immerse 1 g of micro-
Adsorbed moisture ðgÞ
Hygroscopicityð%Þ ¼  100 ð4Þ capsules powder on a surface of 400 mL distilled water at 25 °C
Sample weight ðgÞ
[16].

2.3.6. Bulk density 2.3.12. Solubility

Bulk density of the microcapsules powders was determined Solubility of microcapsules powders was determined according
according to Saifullah et al. [15]. Two g of samples was poured into to Santhalakshmy et al. [13]. One g of microcapsules powder was
a 10 mL graduated measuring glass cylinder, then bulk density was mixed and transferred into 100 mL of distilled water, stirred using
calculated as shown in Eq. (5): 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
Sample weight ðgÞ
Bulk density ðg cm3 Þ ¼ ð5Þ dried at 105 °C. Solubility of the microcapsules powders then was
Sample volume ðcm3 Þ
calculated using Eq. (11):
Weight of the powder ðgÞ in the supernatant
2.3.7. Tapped density Solubilityð%Þ ¼
Weight of the powder ðgÞ in the solution
Tapped density of the microcapsules powders was determined
according to Saifullah et al. [15]. For measuring tapped volume of  100
the samples, 2 g of each sample was placed in a 10 mL graduated ð11Þ
measuring glass cylinder and drop the cylinder gently 100 times
onto a rubber mat from a height of 20 cm. Afterward, the tapped
2.3.13. Color
density was calculated according to Eq. (6):
Color of microcapsules powders was measured using a col-
Sample weight ðgÞ orimeter (HunterLab UltraScan PRO Spectrophotometer, Hunter
Tapped density ðg cm3 Þ ¼ ð6Þ
Tapped volume ðcm3 Þ 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
2.3.8. Particle density
transparent plastic bag, the color parameters [L* (light\dark), a*
Particle density of microcapsules powders was measured
(red\green) and b* (yellow\blue)] were determined in randomly
according to Santhalakshmy et al. [13]. One g of dried powder sam-
three different surfaces of each sample [17].
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
2.3.14. Particle size analysis
was shaken for 30 s. then, the wall of the cylinder was washed with
Particle size of microcapsule powder was determined by using a
2 mL of petroleum ether and the total volume were read. The par-
laser particle size analyzer (Microtrac S3500, Microtrac Inc., North
ticle density was calculated according to Eq. (7):
Largo, FL, USA). Reconstituted microcapsule was prepared through
Particle density ðg cm3 Þ dispersing 1 g of microcapsules powder in 100 mL of distilled
Sample weight ðgÞ water using a magnetic stirrer (500 rpm for 30 min) at 25 °C. The
¼
Total volume of petroleum ether and suspended particles ðcm3 Þ  7 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].
2.3.9. Flowability
2.3.15. Thermal analysis
Flowability of the Fingered citron extract microcapsule powders
Thermal behavior of the microcapsule powder was determined
was estimated based on Carr’s index and Hausner ratio [15].
by using a differential scanning calorimetry (DSC) (DSC Q2000, TA
The Carr’s index (CI) was used to expresses the flow ability of
Instruments, New Castle, DE, USA) according to Hu et al. [19] with
microcapsules powders based on tapped density and bulk density
some modifications. Approximately 5 mg of the microcapsule pow-
[13]. The Carr’s index of the microcapsules powders was calculated
der was heated on an aluminum pan from 25 to 250 °C at a rate of
using Eq. (8):
10 °C/min under the protection of nitrogen atmosphere (50 mL/
Tapped density  Bulk density min).
CIð%Þ ¼  100 ð8Þ
Tapped density
2.3.16. Crystallinity (X-ray diffraction)
Cohesiveness of the microcapsules powders was estimated
Crystallinity of the microcapsule powder was evaluated using
using Hausner ratio (HR) based on tapped density and bulk density
an X-ray diffractometer (D2 PHASER, Bruker AXS Co. Ltd., Karl-
[15]. The Hausner ratio of the microcapsules powders was calcu-
sruhe, Germany) [20]. The scanning region of the diffraction angle
lated using Eq. (9):
(2h) ranged from 5° to 80°. X-ray diffraction patterns of samples
Tapped density were analyzed using software (MDI Jade 6) and calculated as rela-
HR ¼ ð9Þ
Bulk density 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) powders, as shown within Table 3, ranged from 0.47 to
0.60 g cm3. GMS formulation displays the highest tapped density,
Table 2 shows water activity mean values of the Fingered citron followed by MSW formulation. GMW formulation had the lowest
extract microcapsule powders. GMW formulation had the highest tapped density and no significant differences (p  0.05) between
water activity, whilst GMSW formulation had the lowest water mean values of GMSW, and GSW formulations. Tapped density
activity and no significant differences (p  0.05) among moisture mean values of Fingered citron extract microcapsule powders in
content mean values of GMS, GSW, and MSW formulations. As it this study were close to those of the tapped density values already
is depicted within Table 2, water activity of Fingered citron extract reported [25].
microcapsule powders ranged from 0.23 to 0.33. Such values indi-
cates that Fingered citron extract microcapsule powders are con- 3.8. Particle density
sidered stable materials concerning microbial contamination
where water activity values were lower than 0.6. Low water activ- Particle density of Fingered citron extract microcapsule pow-
ity would limit microbial growth, overcome caking problems, ders, as shown within table 3, varied from 1.43 to 1.83 g cm3. Par-
improve physicochemical stability and total acceptability [25]. ticle density mean value of MSW formulation was significantly
lower (p  0.05) compared to those of the other formulations,
3.5. Hygroscopicity while that of GMS formulation was found to be the highest. Particle
density mean values of Fingered citron extract microcapsule pow-
Hygroscopicity is the ability of a material to absorb moisture ders of this research study were found to be higher than (0.7–
from the atmosphere. Hygroscopicity, when it is high would cause 1.2 g cm3) for microencapsulated refined kenaf seed oil [25].
aggregation of the spray dried powder, which affects the nutri-
tional and flow properties of the powder. Hygroscopicity of GMSW
3.9. Flowability
formulation was significantly high (p  0.05) compared to those of
the other formulations. The lowest hygroscopicity mean value was
Carr’s index and Hausner ratio are two closely related empiri-
that of MSW formulation (Table 2). Hygroscopicity mean values of
cally derived parameters that allow assessing flow behavior based
the Fingered citron extract microcapsule powders of this research
on bulk and tapped densities [28]. Results of this research study
study was lower than hygroscopicity values that were reported
showed that Carr’s index mean values were in the range of
in previous studies using gum arabic as wall material, including
27.35–43.59%, indicating poor powder flowability. Hausner ratio
Gagaita fruit extract (14.8–18.8%) [26]. Similar results were
mean values were in the range of 1.38–1.87%, indicating high pow-
reported for microencapsulated refined kenaf seed oil (7.8–10.1%)
der cohesiveness. As it is shown in Table 4, mean values of CI and
[25].
HR for all formulations were high and significantly different
(p  0.05) from each other. GMSW, GSW, and MSW formulations
3.6. Bulk density
were of awful flowing powders. GMW formulation was of very
poor flowing, while GMS formulation was of poor flowing. Powders
Bulk density mean values of the formulations of this research
of all formulations were found of poor flow behaviors, but the pow-
study, as shown in table 3, ranged from 0.28 to 0.44 g cm3. Similar
ders were easily compressible. High mean values of CI and HR indi-
range of bulk density for the microencapsulated powders prepared
cate poor flowability and they are generally related to high values
using spray drying (0.28–0.40 g cm3) have been reported [27].
of the interparticle friction [29]. Microcapsule powders that are
Bulk density of the GMS formulation was significantly high
obtained in this research study were very compressible. Similar
(p  0.05) compared to those of the other formulations, while no
mean values of CI (33.72–48.65%) and HR (1.53–1.96) for microen-
significant differences (p  0.05) among mean values of GMSW,
capsulation of flax oil with zein [30].
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]. 3.10. Porosity

3.7. Tapped density Porosity is an important property in the food industry especially
in the reconstitution of dry powders. The porosity of the powders
Tapped density of powders is a variable that affects the packag- indicates the ratio of the volume of voids between the particles
ing, transportation, and commercialization of powders and indi- and the volume of pores to the total volume occupied by the pow-
cates the weight of powder that can fit in a container. The der [25].
advantage of produce spray dried powders with higher tapped Porosity mean values of Fingered citron extract microcapsule
density is the smaller containers required to store [27]. Tapped powders formulations of this research study ranged from 61.37
density mean values of Fingered citron extract microcapsule 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 Lightness mean values (L*) ranged from 94.62 to 95.61, which indi-
lowest. Mean values of porosity in all formulations in this research cates that all samples tend to be of white color. Mean values of (a*)
study were found to be in agreement with results [31] where the ranged from 0.53 to 0.79, which indicates that all samples tend
porosity mean values ranged from 68 to 75%. High values of poros- to be of green color. GMS formulation had an (a*) mean value that
ity indicate presence of a considerable number of spaces between was found significantly lower (p  0.05) compared to mean values
particles, which hold oxygen that may cause degradation reactions of other formulations. Mean values of (b*) ranged from 7.14 to 9.01
[13]. which indicates that all samples tend to be of yellow color. GMS
formulation had a (b*) mean value that was found significantly
3.11. Wettability lower (p  0.05) compared to mean values of other formulations
and this might be attributed to its high whey protein content.
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 3.14. Particle size analysis
attribute in food processing [25]. Wettability mean values of
microcapsule powders varied from 11.88 to 14.44 min. Wettability Because it affects quality and flowability of final product, parti-
mean values of all formulations carried out in this research study cle size is taken into consideration during powder processing for-
are tabulated in Table 5. Wettability mean value of GMSW formu- mulation. [29]. Appearance, dispensability, and flowability of
lation was the highest, but not significantly different (p  0.05) microcapsule powders are highly influenced by particle size [32].
from those of GMW and MSW. Wettability mean value of GMS for- Mean values of particle size diameter of Fingered citron extract
mulation was the lowest, but not significantly different (p  0.05) microcapsule powders as depicted in Fig. 2 ranged from 14.34 to
from those of GMW and GSW all other means of formulations in 26.47 lm. MSW formulation had the highest particle size, whilst
this research study. No significant differences (p  0.05) were GMW formulation had the lowest particle size and no significant
found among wettability mean values of GMS, GMW and GSW for- differences (p  0.05) among particle size of GMSW, GMS, and
mulations. Range of wettability (11.88–14.44 min) for the micro- GSW formulations were found. Particles size of Fingered citron
capsule powders obtained in this research was wider than the extract microcapsule powders formulated in this research study
range (6–10 min) already reported [25] for refined kenaf seed oil met particle size requirement of a microcapsules food powder
microcapsule powders. (10–100 mm) according to Fang and Bhandari [33]. Distribution
of particle size for reconstituted microcapsule formulations exhib-
3.12. Solubility ited different distribution peaks in a range of 0.26–87.99 lm
(Fig. 3). GMSW and GMW formulations showed a heterogeneous
Solubility is the last particle dissolution step and is a decisive size were they exhibited distribution with two different peaks. Par-
factor for quality of powder that are used as ingredients in food ticle size values of microcapsule powders formulated in this study
industry. Poor soluble powders may cause processing difficulties are consistent with results reported by Fernandes et al. [32].
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].

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 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-
Fig. 3. Particle size distribution curves of rehydrated of the Fingered citron extract tial microbiological instability [35].
microcapsule powders.

3.17. Scanning electron microscopy (SEM)

3.15. Thermal analysis
Microstructures of Fingered citron extract microcapsule pow-
Thermal behavior of Fingered citron extract microcapsule pow- ders are depicted through SEM micrographs shown in (Fig. 6) the
ders evaluated by DSC is presented in Fig. 4. The formulations samples were examined by SEM in order to determine the presence
showed endothermic peaks ranged between 155.85 and 189.47 °C. of fractures, cracks, or any other possible defects that could expose
Optimal thermal stability of Fingered citron extract microcap- since any fracture may lead to the degradation and oxidation of the
sule powders was achieved when GMW formulation was used as exposed encapsulated material [36].
wall materials. GMW formulation was significantly high The micrographs by SEM showed the shape of the microcap-
(p  0.05). Results showed that presence of modified starch in for- sules which appeared spherical, and semi-spherical, though the
mulations negatively affects thermal stability. In presence of mal- typical shape of spray dried particles should be spherical, with a
todextrin however, starch has a positive effect, but whey protein mean size of 10–100 mm [33]. The SEM micrograph also showed
has better effect compared with maltodextrin. Formulations that dents, rough, wrinkled surfaces and slight agglomeration. Frac-
contain gum arabic, whey protein and maltodextrin were found tured microcapsules were observed in powders of GMSW and
of superior thermal stability. MSW formulations, which might be attributed to the low drying
Thermal stability findings in this research study were consistent temperature as well as viscoelastic and film-forming properties.
with the results obtained by Kang et al. [12] who investigated ther- It is apparent that microcapsules had various sizes and that
mal behavior of chlorophylls microcapsules by gum aribic and mal- might be related to an increase in inlet temperature in the spray
todextrin in different ratios. They indicated that thermal stability dryer, as it accelerated the rate of drying of the droplets. It is noted
was improved using gum aribic and maltodextrin as wall materi- that there was some cracks, breaks, and contractions in microcap-
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 Fig. 5. Relative crystallinity by X-ray diffraction patterns of the Fingered citron
the data. extract microcapsule powders.
1132 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134

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,
Fig. 6. Scanning electronic microscopy of the Fingered citron extract microcapsule 1446 cm1, 1390 cm1 (Amide type II, N-H bending) and
powders, (a) GMSW formulation; (b) GMS formulation; (c) GMW formulation; (d) 1064 cm1 (CAO stretching and C-O-H bending). These results
GSW formulation; (f) MSW formulation.
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
sules, where that might be attributed to the high rate of steam gen-
to the CAH stretching from the carboxylic group appeared around
eration and the rapidly crust expanded [10]. Results of SEM analy-
2920 cm1. Peaks corresponding to amine or carbonyl group
sis in this research study were in agreement with those presented
appeared at 1601 cm1 in the GMS formulation around
in previous studies that showed irregular spherical shaped parti-
1635 cm1 in other formulations. Amide ΙΙ (1530 cm1) appeared
cles with many shrinkages and dents on the surface [25–27,32].
in all formulations except GMS formulation, and that might be
Different morphologies and irregular surfaces might be related
attributed to absence of whey protein. Peaks 1150 cm1,
to differences in feeding ratio, droplet size, and temperature
1075 cm1, and 1020 cm1 which corresponding to C-O stretching
through drying process. Shrinkage of the particle followed by an
and C-O-H bending appeared in all formulations [12,19,25,37].
incipient expansion may induce changes in the size of particles
Fingered citron extract spectrum showed an absorption band at
and broken shells. Moreover, the irregularity on the surface of
2935 cm1 which attributed to the asymmetric C-H stretching of
the microcapsules may be desirable in terms of its enhanced dis-
the methyl groups that are present in most of the phenolic com-
persibility and the rehydration of the powders [36].
pounds [37]. It is noticeable that the bands (1973, 2031 and
2165 cm1) appeared in all microcapsules but did not appear in
3.18. Fourier transform infrared spectroscopy (FT-IR)
Fingered citron extract spectra. In addition, the Amide ΙΙ band
(1530 cm1) has not appeared in Fingered citron extract spectra
FT-IR spectra of the raw materials (GA, MD, MS, and WP), the
but it appeared in all formulations that contain whey protein.
microcapsules (GMSW, GMS, GMW, and GSW) and Fingered citron
The spectra of microcapsules and Fingered citron extract confirmed
extract are shown in Fig. 7.
that the microencapsulation by spray drying was successfully
Absorption bands in the spectrum of gum arabic were observed
achieved, where there was no core material on the surfaces of
at 3276 cm1 (OAH stretching), 2919 cm1 (CAH stretching from
the microcapsules.
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]. 4. Conclusions
Maltodextrin spectrum showed absorption bands at 3291 cm1
(OAH stretching), 2920 cm1 (CAH stretching from the carboxylic The microcapsules produced by using gum arabic/maltodex-
group), 1644 cm1 (C@O stretching), 1360 cm1 (OAH bending), trin/modified starch (GMS) was chosen as an optimum encapsula-
and 1150 cm1, 1078 cm1, 1001 cm1 (CAO stretching and tion process due to its superiority in most of the properties, where
CAOAH bending) and this was in agreement with Kang et al. [12]. it provided the highest encapsulation yield and efficiency. More-
 A.A. Mahdi et al. / International Journal of Biological Macromolecules 152 (2020) 1125–1134 1133

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