Powder Technology 386 (2021) 136–143
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Powder Technology
journal homepage: www.elsevier.com/locate/powtec
Microencapsulation of phenolic-enriched extract from cocoa pod husk
(Theobroma cacao L.)
Van Tang Nguyen a,b,⁎, Anh Xuan Tran c, Van Anh Thi Le c
a
Research, Development and Teaching Group on Functional Foods, Nha Trang University, No. 2 Nguyen Dinh Chieu, Nha Trang 57000, Viet Nam
b
Faculty of Food Technology, Nha Trang University, No. 2 Nguyen Dinh Chieu, Nha Trang 57000, Viet Nam
c
Department of Life Science, University of Science and Technology of Ha Noi, Vietnam Academy of Science and Technology, 18 Hoang Quoc Viet, Nghia Do, Cau Giay, Ha Noi, Viet Nam
1. Introduction
Theobroma cacao L. is known to possess originated from Central and
South America. Cocoa was first cultivated in Mexico, South America, and
then spread throughout the Caribbean islands. Currently, West Africa
produces appropriately 75% of world cocoa which becomes their impor-
tant source of export earnings [1]. According to the World Cocoa Foun-
dation in 2016, the world market value of the annual cocoa crop is the
US $5.41 billion. Cultivated cocoa is spilled into 4 varieties: Forastero,
Criollo, Trinitario, and Nacional. In which, Forastero originated from the
Amazon region that is the most generally cultivated species thanks to
its high yield (95% of world cocoa production). Criollo is a smaller
amount widely cultivated since it displays low vigor, poor productivity
and high susceptibility to diseases. Trinitario, a hybrid of Forastero and
Criollo, has the best characteristics from its parents: the high yield of
Forestero, and the refined taste of Criollo. Nacional is the traditional va-
riety of cocoa grown in Ecuador, with unique flavor and aroma, referred
to as “Arriba” [2]. In Vietnam, cocoa trees are mainly grown within the
Central Highlands and Southern provinces. In 2016, cocoa production
of Vietnam is about 2500 tons accounting for below 0.1% of total
world cocoa production.
The cocoa bean constitutes 24–33% of the fresh fruit weight, dropping
67–76% of the fruit as cocoa pod husk (CPH) as a by-product. The CPH
can be potentially applied in many fields such as food processing, cos-
metics manufactory, pharmaceutical production, fuel industry, etc. [3].
However, the CPH has been recently used to manufacture animal feeds
and organic fertilizer, thus their value is underrated and they may be-
come a pollution risk for the environment [4,5]. Some studies showed
that the extract from the CPH contains a high content of phenolic com-
pounds. As stated by Valadez-Carmona et al. (2017) [6], some phenolics
found in the CPH are catechin, quercetin, epicatechin, gallic acid,
coumaric acid and protocatechuic acids, in which catechin accounts for
36% total amount. Bondia-Pons et al. (2009) [7] suggested that phenolic
compounds have good antioxidant activity and anti-inflammatory prop-
erties, which play a significant role in preventing many chronic diseases.
However, phenolic compounds are unstable when exposed to oxygen,
⁎ Corresponding author at: Research, Development and Teaching Group on Functional
Foods, Nha Trang University, No. 2 Nguyen Dinh Chieu, Nha Trang 57000, Viet Nam.
E-mail address: tangnv@ntu.edu.vn (V.T. Nguyen).
https://doi.org/10.1016/j.powtec.2021.03.033
0032-5910/© 2021 Elsevier B.V. All rights reserved.
UV light, temperature, and humidity due to the presence of unsaturated
bonds in their molecular structures [8].
Microencapsulation is an effective technique to enhance the stability
of phenolics. Microencapsulation is the process in which small particles
such as a liquid, or gas can be entrapped within a layer of coating or a
matrix with microscopic size for protecting the coated materials against
adverse reactions and promoting the controlled release of the encapsu-
lates [9]. Choosing the correct coating materials is an important step to
stabilize the micro-particles [10]. Maltodextrin (MD) has been widely
employed in the bioactive compounds microencapsulation due to its
low cost, neutral taste and aroma. Some advantages of MD can be men-
tioned as good film-forming property, high water solubility, low viscos-
ity [11], and great protection against the oxidation of core materials.
Gum Arabic (GA) is a hetero-polysaccharides generally used as wall ma-
terials in microencapsulation. It is defined as a good emulsifier with sev-
eral properties such as non-toxic, odorless, tasteless, and low viscosity
[12]. Chitosan is one of the natural biodegradable groups of polymers
extensively applied in microencapsulation. Besides its good film-
forming ability [13], it has some limits like low solubility in water and
organic solvent, which reduces its exploitation for special functions
[14]. Carrageenans are hydrophilic polysaccharides produced from red
seaweeds (Rhodophyta). Depend on the types of carrageenan (κ, ι,
and λ), it exhibits a wide spectrum of the rheological behavior which
can be applied for microencapsulation [13]. Gelatin derived from colla-
gens by destroying their secondary and higher structure, is still a first
commercially choice as wall material due to its gelling ability, water sol-
ubility, excellent emulsifying property, good film-forming capacity and
high cross-linking activity through its primary amino group, etc. [9,13].
In microencapsulation technology, freeze-drying is often applied for
heat sensitive/labile compounds and high-value products, while spray
drying is normally used for the production of aromas and flavors, and
non-heat sensitive/non-labile compounds [15]. The principle of freeze-
drying is the sublimation under low pressure of ice formed by rapid
freezing and the removal of bound water molecules through the process
of desorption.
The moisture content and water activity of powdered samples are
two factors affecting the chemical reaction and microbiological spoilage
in foods, which impact the stability, shelf-life, and other technical
properties of the powder. During storage, the control sample was
V.T. Nguyen, A.X. Tran and V.A.T. Le Powder Technology 386 (2021) 136–143

hygroscopic faster than the others. The main benefit of wall materials is
to prevent the absorption of moisture from the outside environment,
therefore the moisture content and water activity of the microencapsu-
lated extract is lower and the dehumidification process occurs more
slowly, which prolongs the shelf-life and enhances the quality of
samples.
Solving environmental problems related to agricultural wastes is
a current trend in many countries, and converting wastes to high
value-added products has increasingly got attention nowadays. The
CPH, a by-product of cocoa processing, becomes a threat to environ-
ment due to its large amount. Recovery of natural bioactive com-
pounds from the CPH can reduce its environmental issues and use
to produce functional foods or drugs in order to respond to the
marked increase in carcinogenicity of synthetic compounds and seri-
ous diseases. Several studies on the proximate composition and ex-
traction the phenolic compounds from CPH have been conducted.
However, no studies reported on microencapsulation of CPH extract.
Thus, this study aimed to microencapsulate the CPH extract rich in
phenolic compounds using different combinations of maltodextrin,
gum Arabic, chitosan, carrageenan and gelatin as coating materials
and to evaluate the physiochemical, phytochemical, antioxidant
properties and morphological characteristics of powdered CPH ex-
tract without and with microencapsulation.
extraction time of 30 min and an irradiation time of 5 s/min. After ex-
traction, the extract was quickly cooled to room temperature using
ice water bath and then separated by centrifuging at 4000 rpm for
20 min. Next, the extract was condensed using a vacuum rotary
evaporator at temperature 65 °C, pressure 160 mbar and speed
90 rpm till 10% of the total volume.
2.4. Microencapsulation of CPH extract
Freeze-drying is the technique was employed for the microencapsu-
lation of CPH extract [17,18]. Maltodextrin and its mixtures with gum
Arabic, chitosan, carrageenan or gelatin were investigated as coating
materials. The ratios of coating materials for microencapsulation of
CPH extract were shown in Table 1. At first, the coating materials were
dissolved in water and stored at 4 °C for 1 day to hydrate. After that,
the coating solutions were mixed with the condensed CPH extract at a
ratio of 1:1 (w/w). The mixtures were then homogenized for 20 min
and dried in a freeze dryer at −40 °C and 0.001 mbar for 2 days to obtain
the powdered extract. The powder was stored in a desiccator containing
silica until required (120h).
2.5. Analysis of physiochemical properties of powdered CPH extract without
and with microencapsulation

2. Material and methods 2.5.1. Moisture analysis (MC)

2.1. Plant material
The fresh cocoa pod husk (Theobroma cacao trinitario variety) was
collected from the Thanh Trieu commune, Chau Thanh district, Ben
Tre province, Vietnam (latitude 10.1732°N, longtitude 106.1550°E) on
October 12th, 2019. During transportation to the laboratories at the
Nha Trang University, the CPH was covered by dry ice bags and stored
in a sealed foam container. Briefly, the CPH was chopped into thin slices
(4–5 mm in thickness), packaged in sealed polyamide bags and stored
in a freezer at −20 °C until required. The fresh CPH was naturally
thawed at room temperature and then dried to a constant weight in a
microwave oven at 720 W. During the drying, microwave radiation
time was applied to be 15 s/min and the door was opened for 5 s/min
to release vapor until dried. The dried sample was stored in the freezer
at −20 °C until used.
2.2. Analytical chemicals
All chemicals used in this research were of analytical grade. Absolute
ethanol, chloroform, methanol, Folin–Ciocalteu reagent, sodium car-
bonate, sodium hydroxide, aluminum chloride, vanillin, sulfuric acid,
Bromocresol green, citric acid, disodium phosphate, hydrochloric acid,
2,2′-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), potas-
sium persulfate, 2,2-diphenyl-1-picryl-hydrazil (DPPH), copper (II)
chloride, ammonium acetate, neocuproine, sodium acetate, 2, 4,
6-tripyridyl-s-triazine (TPTZ), iron (III) chloride and assay standards, in-
cluding gallic acid, catechin, escin, atropine and trolox were purchased
from the Sigma-Aldrich (Missouri, United States) and Tokyo Chemical
Industry Co., Ltd. (Tokyo, Japan). All coating materials were of food
grade. Maltodextrin and carrageenan were achieved from HiMedia Lab-
oratories (Maharashtra, India), gum Arabic and gelatin were obtained
from Merck KGaA (Darmstadt, Germany).
The MC of powdered CPH extract without and with microencapsula-
tion was determined by drying it in a hot-air oven (Memmert,
Schwabach, Germany) at 105 °C until constant weight based on the
AOAC official methods of analysis [19].
2.5.2. Water activity (aw) measurement
Aw of powdered CPH extract without and with microencapsulation
was measured at 25 ± 0.5 °C using a water activity meter Rotronic
Hygrolab C1 (Rotronic Instruments Pte Ltd., Bukit Merah Central,
Singapore) [20,21].
2.5.3. Determination of water soluble index (WSI)
Briefly, 0.15 g of powdered CPH extract without and with microen-
capsulation was dissolved in 10 mL distilled water using the vortex
mixer to fasten the solubility. The mixture was then centrifuged
at z4000 rpm for 20 min. The supernatant collected was transferred to
crucibles (pre-weighted) and dried in a hot-air oven (Memmert,
Schwabach, Germany) at 105 °C until a constant weight [20]. The WSI
was calculated according to the following Eq. (1):
TDS
WSI ¼  100 ð1Þ
TDP
where WSI is water soluble index (%); TDS and TDP are total dried su-
pernatant (g) and total dried powder (g), respectively.
Table 1
Ratios of encapsulating materials for microencapsulation of phenolic-enriched CPH
extract.
Samples Encapsulating materials (%)
Maltodextrin Gum Arabic Chitosan Carrageenan Gelatin

2.3. Preparation of CPH extract 0 0 0 0 0 0

1 100 0 0 0 0
2 80 20 0 0 0
Extraction of phenolics from the CPH by MAE was carried out 3 80 10 10 0 0
based on previous research [16]. First, 20 g of dried CPH powder 4 80 10 0 10 0
was soaked in 1 L of distilled water. The flask was put in microwave 5 80 10 0 0 10
oven and heated for 20 s at 600 W three times (5 s apart each Samples 0 to 5 are the CPH extract without microencapsulation (control sample) and with
time). MAE was then applied at a microwave power of 600 W, an microencapsulation.

137
V.T. Nguyen, A.X. Tran and V.A.T. Le
2.5.4. Measurement of pH
The powdered CPH extract without and with microencapsulation
after determining water soluble index was reused by dissolving it in dis-
tilled water and measured pH of solution at room temperature by a pH
meter calibrated with standard pH buffer [20].
2.6. Analysis of phytochemical compounds of powdered CPH extract with-
out and with microencapsulation
2.6.1. Analysis of total phenolic content (TPC)
TPC of powdered CPH extract without and with microencapsulation
was analyzed supported previous study with some modifications
[22,23]. 0.5 mL of extract was mixed with 2.5 mL of 10% (v/v) Folin–
Ciocalteu reagent in distilled water. The mixture was kept to settle for
6 min, then 2 mL of 7.5% (w/v) Na2CO3 solution was added. The absor-
bance of the mixture was measured using a UV-VIS spectrophotometer
at 765 nm after being incubated in the dark at room temperature for 1 h.
Water and gallic acid were used as a control and standard. The TPC was
described as mg gallic acid equivalents (GAE)/g dried sample.
2.6.2. Analysis of total flavonoid content (TFC)
TFC of powdered CPH extract without and with microencapsulation
was performed using the formerly reported method [23,24]. Firstly,
0.5 mL of extract was mixed with 2 mL of distilled water and 0.15 mL
of 5% (w/v) Na2CO3 solution. The mixture was incubated in the dark at
room temperature for 6 min. Next, 0.15 mL of 10% (w/v) AlCl3 solution
was added and the mixture was kept for a further 6 min. Finally, after
adding 2 mL of 4% (w/v) NaOH solution and 0.7 mL of distilled water,
the mixture was incubated for 15 min. The absorbance of the mixture
was measured at 510 nm using a UV-VIS spectrophotometer. Water
and catechin were used as a control and standard, respectively. The
TFC was calculated as mg of catechin equivalents (CE)/g dried sample.
2.6.3. Analysis of total saponin content (TSC)
TSC of powdered CPH extract without and with microencapsulation
was determined according to the prior work [23,24]. Briefly, 0.25 mL of
extract was mixed with 0.25 mL of 8% (w/v) vanillin solution in metha-
nol and 2.5 mL of 72% (v/v) H2SO4 solution. The mixture was incubated
at 70 °C for 15 min and then rapidly cooled using an ice water bath to
room temperature. The absorbance of the mixture was read at 560 nm
using a UV-VIS spectrophotometer. Water and escin were used as con-
trol and standard, respectively. The TSC was quantified as mg of escin
equivalents (EE)/g dried sample.
2.6.4. Analysis of total alkaloid content (TAC)
TAC of powdered CPH extract without and with microencapsulation
was determined using Bromocresol green (BCG) reagent according to
the method reported by Ajanal et al. (2012) [25]. At first, to prepare
BCG solution, 69.8 mg of BCG was dissolved in 3 mL of NaOH 2 N and
5 mL of distilled water, and heated until the solution was completely
dissolved. The solution was then diluted to 1000 mL by distilled water.
The phosphate buffer solution was prepared by adjusting the pH of
2 M sodium phosphate to pH 4.7 with 0.2 M citric acid. 1 mg of pure at-
ropine was dissolved in 10 mL of distilled water to make atropine stan-
dard solution.
Next, the powdered CPH extract without and with microencapsula-
tion were dissolved in HCl 2 N and filtered, then 1 mL of solution was
poured into funnel and washed by 10 mL of chloroform (three times).
The pH of solution was neutralized by NaOH 0.1 N. Then, 5 mL of BCG
solution and 5 mL of phosphate buffer solution were added to the solu-
tion. This mixture was vigorously shaken and completely extracted with
1, 2, 3 and 4 mL of chloroform. The extract were collected in a 10 mL vol-
umetric flask and diluted with chloroform. The absorbance of extract
in chloroform was measured using a UV-VIS spectrophotometer at
470 nm. Water and atropine were used as control and standard,
138
Powder Technology 386 (2021) 136–143
respectively. The TAC was presented as mg atropine equivalents
(AE)/g dried sample.
2.7. Assessment of antioxidant capacity of powdered CPH extract without
and with microencapsulation
2.7.1. Assessment of ABTS radical scavenging capacity (ARSC)
ARSC of powdered CPH extract without and with microencapsula-
tion was measured based on previous study with some modifications
[26,27]. To prepare stock solution, 7.4 mM ABTS+ was mixed with
2.6 mM K2S2O8 in distilled water (ratio 1:1). Then, the solution was in-
cubated in the dark at room temperature for 12 h and stored at −20 °C.
For preparation of a working solution, 1.0 mL of stock solution was di-
luted with 60 mL of methanol 100% to obtain the absorbance of 1.1 ±
0.02 at 515 nm. After that, 0.15 mL of extract was mixed with 2.85 mL
of working solution and incubated in the dark at room temperature
for 3 h. The absorbance of mixture was measured at 734 nm using a
UV-VIS spectrophotometer Methanol and water were used as zero
and control, respectively. Trolox was used as standard. The ARSC was
presented as mg trolox equivalents (TE)/mg dried sample.
2.7.2. Assessment of DPPH radical scavenging capacity (DRSC)
DRSC of powdered CPH extract without and with microencapsula-
tion was assessed based on the previous study with some modifications
[28,29]. Briefly, 0.024% (w/v) DPPH (2,2-diphenyl-1-picrylhydrazyl) in
methanol 100% was prepared to make a stock solution and stored at
−20 °C. To prepare a working solution, 1.0 mL of stock solution was di-
luted with 4.5 mL of methanol. This working solution had absorbance of
1.1 ± 0.02 at 515 nm. 0.15 mL of extract was mixed with 2.85 mL of the
working solution and incubated in the dark at room temperature for 3 h.
The absorbance of mixture was measured at 515 nm using a UV-VIS
spectrophotometer. Methanol and water were used as zero and control,
respectively. Trolox was used as standard. The DRSC are estimated as
mg trolox equivalents (TE)/g dried sample.
2.7.3. Assessment of cupric reducing antioxidant capacity (CUPRAC)
CUPRAC of powdered CPH extract without and with microencapsu-
lation was determined based on the former report [28,29]. Briefly, 1 mL
of CuCl2 10 mM solution in distilled water was mixed with 1 mL of
NH4Ac 7.7% (w/v) solution in distilled water and 1 mL of 7.5 mM
neocuproine solution in ethanol 100%. Then, 1.1 mL of extract was
added to the prepared solution and incubated in the dark at room tem-
perature for 1.5 h. The absorbance of mixture was read at 450 nm using
a UV-VIS spectrophotometer. Water and trolox were used as control
and standard, respectively. The CUPRAC was calculated as mg trolox
equivalents (TE)/g dried sample.
2.7.4. Assessment of ferric reducing antioxidant power (FRAP)
FRAP of powdered CPH extract without and with microencapsula-
tion was determined based on the former report with some modifica-
tions [28,29]. Three regents prepared included 300 mM acetate buffer
solution at pH 3.6 (reagent A); 10 mM TPTZ solution in 40 mM HCl (re-
agent B); and 20 mM FeCl3·6H2O solution (reagent C). Prior to use, re-
agents A, B, and C were mixed at a ratio of 10:1:1 to make a fresh FRAP
solution. 0.15 mL of extract was mixed with 2.85 mL of the fresh FRAP
solution and incubated in the dark at room temperature for 30 min.
The absorbance of mixture was measured at 593 nm. Water and trolox
were used as control and standard, respectively. The FRAP were calcu-
lated as mg trolox equivalents (TE)/g dried sample.
2.8. Microstructural analysis of powdered CPH extract without and with
microencapsulation
The outer structure of powdered CPH extract without and with mi-
croencapsulation was visualized by a scanning electron microscope
(SEM) (JSM IT200, JEOL Ltd., Tokyo, Japan). The samples were mounted
V.T. Nguyen, A.X. Tran and V.A.T. Le
onto a sample holder with double-adhesive conducting tapes and
coated with gold particles in a vacuum chamber. The morphology ob-
servation was examined at different magnifications using SEM operat-
ing at an accelerating voltage of 5 kV [20].
2.9. Statistical analysis
Each experiment was conducted in triplicate and all values were
shown as means ± standard deviations. All statistical analyses were
performed using the IBM SPSS Statistics 22 software. Duncan's multiple
range test was used to compare the means with the significant differ-
ence defined below 5% (p < 0.05).
3. Results and discussion
3.1. Physiochemical properties of microencapsulated CPH extract
The physicochemical properties (moisture content, water activity,
water soluble index and pH) of microencapsulated powders from the
CPH with different encapsulating materials is represented in Table 2.
These properties affect directly the quality and storage time as well as
the potential application for further research.
The moisture content of control sample is highest (12.21%) com-
pared to microencapsulated samples (4.51–7.13%). The one-way analy-
sis of variance shows that all microencapsulated samples (from sample
1 to sample 5) were significant differences from the control sample
(p < 0.05). This may be due to the addition of the encapsulating mate-
rials increased the total feed solids and thus, reduced the total moisture
for evaporation [30]. Freeze-dried final products contain extremely low
levels of moisture (1–4%) [31]. However, the rapid freezing due to freez-
ing temperature less than -40 °C results in smaller pores in the outer
layer, which may hinder mass transfer and act as a barrier against sub-
limation, resulting in increased moisture retention [32]. Papoutsis et al.
(2018) [11] found the moisture content varied from 1.15% to 2.15% for
micro-particles from citrus by-product with maltodextrin, soybean pro-
tein, and ι- carrageenan; while Kuck & Noreña (2016) [32] reported the
moisture content ranging from 7.65% to 8.06% for Bordo grape skin mi-
croencapsulated with gum Arabic, polydextrose, and partially hydro-
lyzed guar gum by freeze-drying. Significant differences between
microencapsulated samples were obtained due to the differences in
chemical structure and molecular weight between these encapsulating
materials. The moisture content of sample 3 was the highest among 5
microencapsulated samples (7.13%) due to water-holding capacity of
chitosan. Ul-Islam et al. (2011) [33] showed the increase in water hold-
ing capacity of bacterial cellulose after chitosan treatment. Sample 5 had
the second highest moisture content (6.20%) due to amount of gelatin in
the mixture. Correia et al. (2017) [34] have shown that the higher the
protein content, the higher the moisture in the final powder, due to
the higher water-holding capacity of protein in its amorphous state.
The lowest moisture content (4.51%) was found for sample 1 with
Table 2
Physicochemical properties of phenolic-enriched CPH extract without and with microencapsulation.
Samples Physicochemical properties
Moisture content (%)
0 12.21 ± 0.84a
1 4.51 ± 1.06c
2 4.77 ± 0.33c
3 7.13 ± 0.76b
4 6.17 ± 1.29bc
5 6.20 ± 1.01bc
Samples 0 to 5 are the CPH extract without microencapsulation and being microencapsulated by maltodextrin; maltodextrin and gum Arabic (8:2 w/w); maltodextrin, gum Arabic and
chitosan (8:1:1 w/w); maltodextrin, gum Arabic and carrageenan (8:1:1 w/w); and maltodextrin, gum Arabic and gelatin (8:1:1 w/w), respectively. Values with different letters in the
same column indicate significant differences between samples (p < 0.05).
Powder Technology 386 (2021) 136–143
maltodextrin, which is less hygroscopic due to its high molecular
weight.
The water activity of extract from the CPH was decreased after mi-
croencapsulation. Of which, the water activity of control sample was
0.46, while the water activity of microencapsulated samples (samples
1–5) was 0.44, 0.41, 0.43, 0.41, and 0.42, respectively. Despite of the
lowest moisture content, sample 1 had the highest water activity
(0.44). Maltodextrin is not surface-active and therefore has very poor
emulsifying capacity. In order to form stable emulsions, maltodextrin
is generally mixed with other wall materials such as gum Arabic [35].
Sample 4 has the lowest water activity (0.41) and no significant
difference with water activity of sample 2 (0.41). The higher the water
activity, the more the free water, which has a negative impact on the
shelf-life of the product. The lowest limit of water activity for microbial
proliferation is 0.6 [36]. Therefore, the water activity values of all micro-
encapsulated samples were within the expected range for powdered
products to ensure microbial safety. The water activity of freeze-dried
phenolic-enriched extract from the CPH is higher than the water activity
of Bordo grape skin microencapsulated (about 0.3) [32]. Hussain et al.
(2018) [14] reported that the water activity of polyherbal formulation
microencapsulated using freeze-drying was 0.31–0.45.
Regarding water soluble index (WSI), the solubility of all microen-
capsulated samples was ranged from 64.49 to 94.48%. The WSI of the
final products may be associated with the solubility of wall materials.
The solubility of control sample (92.81%) was significantly higher than
sample 3 (64.49%) and sample 5 (88.86%). The lowest solubility value
was observed for sample 3 with combination of maltodextrin, gum Ar-
abic and chitosan due to low solubility prospective of chitosan [14].
Sample 5 with combination of maltodextrin, gum Arabic and gelatin
had lower solubility than sample 1, 2 and 4. This finding is supported
by Pudziuvelyte et al. (2020) [37] who showed that the solubility of
samples treated with gum Arabic and gelatin was lower than that
treated with maltodextrin and gum Arabic. The solubility in this study
was higher than solubility in the research of Kuck & Noreña (2016)
[32] about grape skin extract microencapsulated by freeze-drying
(85.96–88%).
The pH of CPH extract did not significantly change after microencap-
sulation. Moreover, pH values of microencapsulated samples were not
affected by the different encapsulating agents. Šturm et al. (2019) [12]
showed ratios of maltodextrin and gum Arabic did not impact pH of mi-
croencapsulated propolis extract by freeze-drying. Most bacteria are
neutrophiles and develop well in the pH range of 5.5–8.5, so that bacte-
ria are mostly inhibited or destroyed in high acidic as well as basic envi-
ronments. Table 2 shows that microencapsulated CPH extract were
slightly acidic and the pH of the samples was in the range of
5.28–5.35, hence they could inhibit the growth of bacteria.
3.2. Phytochemical compounds of microencapsulated CPH extract
Fig. 1 shows the physicochemical compounds of CPH extract before
(sample 0) and after microencapsulation (samples 1–5) in terms of
Water activity Water solubility index (%) pH
0.46 ± 0.02a 92.81 ± 5.02ab 5.28 ± 0.03a
0.44 ± 0.01ab 91.40 ± 1.09ab 5.31 ± 0.01a
0.41 ± 0.01c 93.95 ± 1.13a 5.30 ± 0.01a
0.43 ± 0.02bc 64.49 ± 0.85c 5.35 ± 0.10a
0.41 ± 0.01c 94.48 ± 0.69a 5.29 ± 0.01a
0.42 ± 0.01bc 88.86 ± 1.81b 5.28 ± 0.01a
139
V.T. Nguyen, A.X. Tran and V.A.T. Le
Fig. 1. Phytochemical compounds of phenolic-enriched CPH extract without and with microencapsulation. Samples 0 to 5 are the CPH extract without microencapsulation and being
microencapsulated by maltodextrin; maltodextrin and gum Arabic (8:2 w/w); maltodextrin, gum Arabic and chitosan (8:1:1 w/w); maltodextrin, gum Arabic and carrageenan (8:1:1
w/w); and maltodextrin, gum Arabic and gelatin (8:1:1 w/w), respectively. GAE: gallic acid equivalents, CE: catechin equivalents, EE: escin equivalents, AE: atropine equivalents.
total phenolics content (TPC), total flavonoids content (TFC), total sapo-
nins content (TSC), and total alkaloids content (TAC). Regarding the phe-
nolic compounds, the TPC values were significantly decreased for all
microencapsulated samples (9.00 to 15.51 mg GAE/g dried sample) com-
pared to the control sample (29.01 mg GAE/g dried sample). The reten-
tion of phenolic compounds in the microencapsulated powders from
the CPH ranged from 31.03% to 53.45%. The retention of phenolics in
this study was much lower when compared to the retention percentages
in the microencapsulated grape skin extract (81.40–93.50%) [32]. How-
ever, the low retention of phenolic compounds (41.49–61.77%) was
found in the spent coffee ground extract microencapsulated using malto-
dextrin and gum Arabic. As can be seen in Fig. 1, there was no statistically
significant differences between maltodextrin (sample 1) and mixture of
maltodextrin and gum Arabic (sample 2). The TPC of sample 1 using
maltodextrin was 15.51 mg GAE/g dried sample with microencapsula-
tion efficiency of 53.45%, while using gum Arabic in combination with
maltodextrin for sample 2, the TPC was 15.19 mg GAE/g dried sample
with encapsulating efficiency of 52.35%. The high TPC retention in sam-
ples 1 and 2 was mainly attributed to the ratio of maltodextrin in the
mixture of coating material. Gum Arabic is a hetero-polymer formed of
dense branches of sugar, consisting of low quantity of protein (< 3%)
[12], which connect to the carbohydrate skeleton via covalent bonds,
proceeding as a remarkable carrier material. Ratio of gum Arabic in sam-
ple 2 was higher than in sample 3, 4 and 5 (Table 1), which led to signif-
icant differences in TPC between these samples. Carrageenans are highly
polydisperse with a polydispersity index of 3 [13], which may form het-
erogeneous size of micro particles and lower the phenolic retention of
sample 4. Sample 3 with mixture of maltodextrin, gum Arabic and chito-
san (8:1:1 w/w) had the lowest retention of phenolics (31.03%). The
function of the coating material may have the most effect on the stability
of phenolic compounds. In freeze-drying process, the crushing of the
freeze-dried products may increase the surface exposure to oxygen,
which induces the occurrence of oxidation reactions, and hence lead to
degradation of compounds. Furthermore, the type and concentration of
wall materials may also affect the phenolics degradation.
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Powder Technology 386 (2021) 136–143
The TFC values of microencapsulated CPH extract were varied from
13.10 to 24.96 mg CE/g dried sample and significantly lower than con-
trol sample (49.93 CE/g dried sample). Sample 1 microencapsulated
with maltodextrin obtained the highest retention of flavonoids
(49.99%), while sample 3 obtains the lowest retention of flavonoids
(26.24%). Ballesteros et al. (2017) [8] reported the retention flavonoid
percentage of the microencapsulated spent coffee ground extract was
varied from 32.57% to 73.53%, while Papoutsis et al. (2018) [11] found
the higher flavonoid retention (56.53–74.40%) from the citrus by-
product extract by freeze-drying using combination of maltodextrin
with soybean protein and ι-carrageenan. The one-way analysis of vari-
ance indicates that there was not significant differences in TFC values
of sample 1, 2, 4 and 5. Papoutsis et al. (2018) [11] has shown the similar
TFC values between microencapsulated sample with maltodextrin
(0.33 ±0.00 mg CE/g dry weight) and microencapsulated one with mix-
ture of maltodextrin and ι-carrageenan (0.33 ± 0.002 mg CE/g dry
weight). Sample 3 with the lowest retention of TFC suggested that chi-
tosan was not the suitable encapsulating agents for the microencapsula-
tion of CPH extract. The reason for this may due to the high water
solubility of maltodextrin may increase the solubility of flavonoids in
solvent, while the low solubility of chitosan in water can lead to limited
releasing the flavonoids in solvent [11,13].
Besides the phenolic compounds, saponins and alkaloids are popular
bioactive compounds found in plants. Saponins are second metabolites
with many potential health benefits. Previous literature reported that
saponins have some pharmaceutical properties such as antioxidant, an-
tibacterial and anti-inflammatory activities, especially anticancer [38].
Alkaloids are well-known bioactive compounds in cocoa, including caf-
feine and theobromine. Along with antioxidant and anti-inflammatory
activity, alkaloids can prevent cancer, cardiovascular diseases, diabetes,
obesity and treat infectious diseases [39]. Therefore, research on TSC
and TAC was to obtain more information about antioxidant compounds
of microencapsulated CPH extract.
The TSC of microencapsulated CPH extract was in the range of
282.23–307.13 mg EE/g dried sample. Of those, the highest saponin
V.T. Nguyen, A.X. Tran and V.A.T. Le
content obtained by sample 2 and the lowest saponin value obtained by
sample 3. This is also due to the high water solubility of maltodextrin
may enhance the solubility of saponins in solvent, whereas the low sol-
ubility of chitosan in water can prevent the saponins to release in sol-
vent [11,13]. The retention of saponins after microencapsulation
(72.94–79.37%) was higher than the retention of TPC (31.03–53.45%)
and TFC (26.24–49.99%). These results are higher than those obtained
by Tan et al. (2015) [40] for bitter melon extract microencapsulation
with different ratios of maltodextrin to gum Arabic (41.70–64.00%) by
spray-drying; the retention of saponin significantly increased when
the ratios of maltodextrin to gum Arabic increased. The high tempera-
ture in spray-drying can lead to the degradation of saponin and lower
the retention of TSC in spray-dried bitter melon extract microencapsu-
lated powders compared to retention of CPH microencapsulated pow-
ders by freeze-drying.
The retention of alkaloids in the microencapsulated CPH powders
ranged from 91.66% to 97.80% and there were no significant differences
between control sample and all microencapsulated samples. The
highest value of alkaloids was obtained by sample 1 (494.55 mg AE/g
dried sample), followed by sample 2 (485.40 mg AE/g dried sample)
and sample 4 (484.65 mg AE/g dried sample). The lowest TAC was ob-
tained by sample 5 (463.47 mg AE/g dried sample). The TAC of microen-
capsulated CPH extract in this study was not affected by different wall
materials and their mixture, and thus the TAC may not impact on the
antioxidant capacity of CPH microparticles. The retention of TAC was
the highest compared to the retention of TPC, TFC and TSC possibly
due to the strong interaction between alkaloids and encapsulating ma-
terials. Furthermore, there was no literature review on microencapsula-
tion of CPH and the effect of wall materials on the TAC.
3.3. Antioxidant capacity of microencapsulated CPH extract
The antioxidant capacity of microencapsulated CPH extract in terms
of ABTS/DPPH radical scavenging capacity (ARSC/DRSC), and cupric/fer-
ric reducing antioxidant capacity (CUPRAC/FRAP) is presented in
Table 3. The freeze-dried CPH extract had higher DRSC, ARSC, FRAP
and CUPRAC values compared to the freeze-dried microencapsulated
CPH extract. The highest level of DRSC was obtained by sample 4
(28.72 mg TE/g dried sample), which was significantly higher than sam-
ple 3 and 5 (19.29 and 23.56 mg TE/g dried sample, respectively). The
DRSC of sample 1 and 2 had no significant differences with sample 4.
The retention percentages of DRSC ranged from 32.62% to 48.56%.
Kuck & Noreña (2016) [32] reported the similar retention of
DRSC (39.67–59.10%) for microencapsulation of grape skin extract;
while Hussain et al. (2018) [14] found a little higher retention
Table 3
Antioxidant capacity of phenolic-enriched CPH extract without and with
microencapsulation.
Samples Antioxidant capacity
DRSC ARSC FRAP CUPRAC
(mg TE/g DS) (mg TE/g DS) (mg TE/g DS) (mg TE/g DS)
0 59.14±1.08a 102.96±1.90a 66.20±1.23a 138.09±0.87a
1 28.35±1.10b 49.16±0.63b 41.78±1.34c 83.41±0.42b
2 28.42±1.65b 42.65±0.88c 39.55±1.37d 78.10±0.39c
3 19.29±0.52d 25.48±0.10e 43.63±0.64bc 60.68±0.93e
4 28.72±1.57b 42.63±2.00c 39.23±1.02d 77.80±0.49c
5 23.56±0.85c 30.68±1.71d 44.43±1.09b 65.60±0.75d
Samples 0 to 5 are the CPH extract without microencapsulation and being microencapsu-
lated by maltodextrin; maltodextrin and gum Arabic (8:2 w/w); maltodextrin, gum Arabic
and chitosan (8:1:1 w/w); maltodextrin, gum Arabic and carrageenan (8:1:1 w/w); and
maltodextrin, gum Arabic and gelatin (8:1:1 w/w), respectively. Values with different let-
ters in the same column indicate significant differences between samples (p < 0.05).
DRSC: DPPH radical scavenging capacity, ARSC: ABTS radical scavenging capacity, FRAP:
ferric reducing antioxidant power, CUPRAC: cupric reducing antioxidant capacity, TE:
trolox equivalents, DS: dried sample.
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Powder Technology 386 (2021) 136–143
(38.65–63.77%) in polyherbal formulation microencapsulated with
gum Arabic, gelatin and maltodextrin. The results indicated that the mi-
croencapsulated samples with higher TPC showed stronger free radical-
scavenging capacity. Sample 3 with the lowest TPC value obtained the
lowest DRSC value due to the presence of chitosan. These findings sug-
gested that phenolics have a main role to antioxidant capacity in the ex-
tract from CPH. Moreover, the high correlation was also found between
DRSC and TFC and SC. However, TAC values had insignificantly influence
the DRSC of microencapsulated CPH extract.
The antioxidant activity of microencapsulated powders by ARSC
assay obtained from 25.48 to 49.16 mg TE/g dried sample; and the re-
tention of ARSC varied in the range of 24.75 to 47.75%, with the
highest values for sample 1, followed by sample 2 and sample 4,
and no significant differences was observed between them. The low-
est value was obtained by sample 3 with the combination of malto-
dextrin, gum Arabic and chitosan. Sample 3 always obtained the
lowest antioxidant components among all microencapsulated pow-
ders. Similar to DRSC, the higher phenolics contents, the stronger of
ARSC. There was strong correlation between ARSC and antioxidant
components of microencapsulated CPH powders. The retention in
this study is much lower when compared to the retention
(61.97–86.7%) in the research of Hussain et al. (2018) [14] about mi-
croencapsulation of polyherbal formulation.
The FRAP assay measures the reducing potential of an antioxidant
reacting with a Fe3+ TPTZ complex (colorless complex) and producing
Fe2+-tripyridyltriazine (blue colored complex) at low pH. The FRAP
values of the microencapsulated CPH extract were varied from 39.55
to 44.43 mg TE/g dried sample and the retention of FRAP ranged from
59.27% to 67.11%. The highest FRAP value was found for sample 5,
followed by sample 3, and no significant differences in FRAP between
them, while the lowest FRAP values was observed for sample 4. Al-
though, sample 3 and 5 resulted in lower TPC and TFC compared to
the others, they obtained the highest FRAP values, which showed that
FRAP may not depend much on the phenolic and flavonoid content.
Papoutsis et al. (2018) [11] found the similar retention percentages of
FRAP in citrus by-product microencapsulated by freeze-drying
(61.74–63.07%), while Ballesteros et al. (2017) [8] found the FRAP re-
tention in spent coffee ground microencapsulated with maltodextrin
and gum Arabic was 56.28–73.49%.
For the antioxidant activity by CUPRAC, the highest value was found
for sample 1 and the lowest value was observed for sample 3, the
CUPRAC retention was in the range of 43.94–60.40%. The results ob-
tained are strongly linear with the TPC, TFC and SC values. Sample 1, 2
and 4 showed the higher antioxidant capacity, and thus provided a
good defense system against oxidation. Kuck & Noreña (2016) [32]
found the higher CUPRAC retention (73.16–78.27%) in grape skin aque-
ous extract microencapsulated with the combination of partially hydro-
lyzed guar gum, gum Arabic and polydextrose. CUPRAC assay measures
the absorbance of Cu(I)-neocuproine chelate formed as a result of the
redox reaction of chain-breaking antioxidants with Cu(II)-neocuproine.
A similar reason is also given for this finding due to the high water
solubility of maltodextrin may promote the solubility of antioxidants
(phenolics, flavoloids and saponins) in solvent, whereas the low solubil-
ity of chitosan in water can lead to limited releasing the antioxidants in
solvent [11,13].
3.4. Microstructural of microencapsulated CPH extract
The structural characteristics of all microencapsulated samples by
freeze-drying had irregularly shaped and various sizes (Fig. 2). Freeze-
dried sample commonly has a glass broken and rigid structure [14,32].
The structural rigidity and irregular shape of freeze-dried sample may
strongly protect the core materials against pressure, heat and light.
The CPH microencapsulated powders had different structures from the
control sample. As can be seen in Fig. 2.1, the surface morphology of
control sample showed the hygroscopic nature of CPH extract. The
V.T. Nguyen, A.X. Tran and V.A.T. Le
Fig. 2. Scanning electron micrographs of phenolic-enriched CPH extract without and with microencapsulation. Samples 0 to 5 are the CPH extract without microencapsulation and being
microencapsulated by maltodextrin; maltodextrin and gum Arabic (8:2 w/w); maltodextrin, gum Arabic and chitosan (8:1:1 w/w); maltodextrin, gum Arabic and carrageenan (8:1:1
w/w); and maltodextrin, gum Arabic and gelatin (8:1:1 w/w), respectively.
porous structure of microencapsulated samples happened due to subli-
mation of ice crystals during freeze-drying. The surface of freeze-dried
samples is completely different compared with the spray-dried micro-
particles. The common structure of spray-dried powders observed is
spherical structures without cracks or fissures, which is similar to the
structure reported by Kuck & Noreña (2016) [32] and Papoutsis et al.
(2018) [11].
The sticky structure of microencapsulated samples was observed
possibly due to their hygroscopicity. When observing the change of
samples in a period of time, all microencapsulated samples was hygro-
scopic after 30 min, while the control sample absorbed moisture after
five min. Due to low moisture content, freeze-dried samples may easily
absorb moisture and the grinding of freeze-dried samples can increase
the exposure to atmosphere. Further, the structure of freeze-dried sam-
ples may be impacted by homogenization that is step to form homoge-
neous matrices around core materials. Time and speed are two main
factors affecting homogenization step. Adjustment of suitable time
and speed may improve the structure of freeze-dried samples.
4. Conclusions
The CPH extract rich in phenolic compounds is a potential source to
utilize in food industry for development of functional foods. The CPH ex-
tract need to be microencapsulated to prolong their shelf-life and pre-
serve their antioxidant properties. The composition of encapsulating
agents has a significant effect on physicochemical properties, retention
of phenolic compounds and antioxidants of CPH extract. The combina-
tion of MD and GA (8:2 w/w) obtained the best characteristics in
terms of low moisture content and water activity, high solubility, high
retention of TPC, TFC, SC, TAC and antioxidant capacity (ARSC, DRSC,
CUPRAC and FRAP). However, further studies are necessary to improve
the structure of freeze-dried CPH extract and to reduce production cost
and processing time.
142
Powder Technology 386 (2021) 136–143
Funding
This work was funded by the Ministry of Education and Training,
Vietnam (MOET) through a research project “Extraction of some key
bioactive compounds from cocoa pod husk for application in functional
foods” to Van Tang Nguyen [grant number B2019-TSN-07].
Credit author statement
Van Tang Nguyen: Conceptualization, Data curation, Formal analy-
sis, Funding acquisition, Investigation, Methodology, Project adminis-
tration, Resources, Software, Supervision, Validation, Visualization,
Writing - original draft, Writing - review & editing. Anh Xuan Tran:
Investigation, Validation, Visualization, Writing - original draft.
Van Anh Le Thi: Supervision, Writing - review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
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