Powder Technology 394 (2021) 562–574

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Powder Technology

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

Choosing the appropriate wall materials for spray-drying

microencapsulation of natural bioactive ingredients: Taking phenolic
compounds as examples
Wangxing Lu, Xing Yang, Jian Shen, Zongze Li, Songwen Tan, Wenjie Liu ⁎, Zeneng Cheng
Xiangya School of Pharmaceutical Sciences, Central South University, Changsha, Hunan 410013, China

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

Article history: Phenolic compounds constitute important parts of natural bioactive ingredients due to their various biological ac-
Received 14 August 2020 tivities. However, phenolic compounds are to some extent restricted by low solubility, poor stability, unpleasant
Received in revised form 20 July 2021 taste and low bioavailability. Spray-drying microencapsulation is an effective strategy to ameliorate or even
Accepted 27 August 2021
tackle such problems and it is crucial to choose optimal wall materials which may affect functional properties
Available online 02 September 2021
of the encapsulated components. In this review, we first described and discussed the physicochemical character-
Keywords:
istics of commonly used wall materials for spray drying. Then we summarized the work done in past 16 years
Microencapsulation about the microencapsulation of phenolic compounds including anthocyanidin, curcumin, catechins, gallic
Spray drying acid, and resveratrol using spray drying is reviewed with a focus on the role of wall materials. Furthermore, we
Wall materials propose some targeted encapsulation strategies for different bioactive ingredients to explore their applications.
Phenolic compounds Finally, we intend to encourage more research in rational selection of the wall materials.
© 2021 Elsevier B.V. All rights reserved.

1. Introduction
Recently, the utilization of natural plant extracts or their bioactive
ingredients for health promotion has become an increasing trend, due
to their link between nutrition and medicine. Natural bioactive ingredi-
ents are those substances that can bring about beneficial health effects
through cellular activities as well as physiological activities [1], and phe-
nolic compounds are one of the most popular natural bioactive ingredi-
ents because of their potential health benefits. Incorporation of natural
bioactive ingredients into various functional food systems is a major
approach to improve their nutritional value. However, there are also
many difficulties encountered limiting their applications, including:
Abbreviations: C, core material; W, wall material; EE, encapsulation efficiency; Cmax,
the average peak concentration; MD, maltodextrin; RMD, resistant maltodextrin; GA,
gum arabic; CP, Capsul™; TS, tapioca starch; GE, gelatin; OSA, octenyl succinic
anhydride modified starch; TP, tricalcium phosphate; CTG, cashew tree gum; CD, b-
cyclodextrin; FG, fenugreek gum; MCC, microcrystalline cellulose; IN, inulin; PEC, pectin;
GG, guar gum; AF, agave fructan; HPAF, high performance agave fructans; HDPAF, high
degree of polymerisation agave fructans; WPI, whey protein isolate; PPI, pea protein
isolate; WPC, whey protein concentrates; SC, sodium caseinate; PHGG, partially
hydrolyzed guar gum; PD, polydextrose; CS, chitosan; HPSC, hydrogenated soy
phosphatidylcholine; G, glucose; DGS, dried glucose syrup; DPPC, dipalmitoyl
phosphatidylcholine; HA, hyaluronic acid; SRAS, Shellac resin ammonium salts; COL,
collagen; MC, micellar caseins; OSCD, octenylsuccinated corn dextrin; BRF, brown rice
flour; NR, Not reported.
⁎ Corresponding author.
E-mail address: wenjie.liu@csu.edu.cn (W. Liu).
(i) conditioned solubility, (ii) inferior stability, (iii) unpleasant taste,
and (iv) limited bioaccessibility and bioavailability [2].
Microencapsulation, which has been employed as a promising tech-
nique to package natural bioactive ingredients, is a widely used eco-
nomical strategy to alleviate these limitations. It is defined as the
entrapment of a substance (core material) within an immiscible sub-
stance (wall material) [3], which can build a barrier to protect the
core material away from undesirable surrounding conditions and en-
hance the beneficial properties, bioavailability and efficacy. Various
techniques, including spray drying, freeze drying, fluid bed coating,
ionic gelation, thermal gelation, emulsion and so on, have been applied
for microencapsulation and each technique presents unique advantages
and disadvantages [4]. The selection of a microencapsulation technique
depends upon encapsulation efficiency, complexity in procedure, pro-
cess cost and the choice of wall materials.
Although most commonly considered as a dehydration process, spray-
drying is also a pervasive and sound technology for microencapsulation
[5]. Compared to other microencapsulation methods, spray drying possess
the benefits of simple operation and low cost. And it is suitable for heat-
sensitive substances like phenolic compounds, as the spray drying temper-
ature is relatively low (generally the inlet temperature is lower than
200 °C) and the residence time of the droplet/particles is very short (in a
matter of seconds). The cooling effect caused by the solvent evaporation
helps the temperature of the dried product does not rise above its wet
bulb temperature [6]. Spray drying involves complex interactions of equip-
ment components, physical properties of feed, and processing parameters

https://doi.org/10.1016/j.powtec.2021.08.082
0032-5910/© 2021 Elsevier B.V. All rights reserved.
W. Lu, X. Yang, J. Shen et al.
[7,8], which all have influence on the final product characteristics. It is
noteworthy that the difference in drying characteristics between wall ma-
terials and core compounds rules this microencapsulation process [9],
which is possible to affect the powder properties like size, shape, flow-
ability, compressibility, bulk density, stability, solubility, process efficiency,
moisture content and the degree of protection for the core material. In a
word, the wall composition and the microencapsulation techniques may
determine functional properties and potential applications of the encapsu-
lated components [10]. In this sense, the main focus of microencapsulation
of natural bioactive ingredients is the improvement of their encapsulation
efficiency, bioavailability or nutrition value by selecting and modulating
the type and proportion of wall materials in the spray drying process.
The application of spray drying for microencapsulation has experienced
an appreciable increase since the late 1950s. Taking phenolic compounds
as an example, the proportion of papers related to spray drying microen-
capsulation of phenolic compounds significantly increased over the past
15 years, and the percentage of published papers increased from 0.43%
in 2004 to 9.07% in 2019, with an almost 210% growth.
2. Phenolic compounds
Phenolic compounds, ubiquitous in plants metabolites, are an
important part of natural bioactive compounds that are widely used
Table 1
Classification of natural phenolic compounds.
Regimentation Examples
Phenolic acids
Flavonoids
Stilbenes
Curcuminoids
Powder Technology 394 (2021) 562–574
for functional foods, nutraceuticals and pharmaceuticals [11,12]. A
large amount of research data indicates that phenolic compounds pos-
sess a high spectrum of biological activities, including antioxidant,
anti-inflammatory, anti-allergenic, antibacterial, antiviral, and even
antitumor functions [13–15]. Therefore, some researchers have related
an inverse association between these biological activities and the inci-
dence of diseases, such as diabetes mellitus, cardiovascular diseases,
and cancer [16].
Phenolic compounds refer to the structure that the hydrogen atoms
on benzene ring in the aromatic hydrocarbon are substituted by
hydroxyl group, and can be classified into monohydric phenol (such
as phenolic acids) and polyhydric phenol (such as stilbenes and flavo-
noids) according to the number of hydroxyl groups in the molecule
[17]. Most of the phenolic compounds are extracted from various plants,
which are called natural phenolic compounds or endogenous phenols
(the rest are exogenous phenols). The examples of different natural
phenolic compounds are listed in Table 1. They can be found in a large
group of plant sources, including legumes, fruits, vegetables, cereals, oil-
seeds, plant oils, tree nuts, herbs and spices [18], and are of significant
amounts in some plant-derived foods [19]. Anthocyanidin, curcumin,
catechins, gallic acid, and resveratrol are important examples of natural
bioactive ingredients from phenolic compounds that are used as color-
ants, antioxidants or nutraceuticals.
Sources Critical properties
soluble in water; sensitive to alkaline pH and oxidation,
berries, tea, wheat
relatively stable under normal conditions
slightly soluble in water; sensitive to oxidation, light and pH;
tea
astringent and bitter; metabolism in the gastrointestinal tract
soluble in water; natural pigments; sensitive to
fruits, flowers
temperature, oxidation, pH, and light
poor solubility; sensitive to oxidation and light;
peanut, cacao
astringent and bitter; rapid metabolic elimination
turmeric poor solubility; sensitive to light; rapid metabolic elimination
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The effectiveness of phenolic compounds depends on their bioactiv-
ity, bioavailability, and stability [20]. However, most of the phenolic
compounds have poor solubility, limited bioavailability and high sensi-
tivity to environmental conditions during processing and storage (oxy-
gen, light, pH, temperature, humidity etc.) [21,22]. Another problem of
phenolic compounds is their unpleasant taste or olfaction, which limits
their application [23]. Moreover, most of the evidences about beneficial
effects of phenolic compounds are derived from experiments performed
in vitro or in animal models [24], and the effective concentrations are
generally magnitude higher than the levels measured in vivo. Even
though a phenolic compound has strong biological activities in vitro, it
might have little biological activity in vivo due to its un-targeted release
[25]. Consequently, it is not only important to know the physicochemi-
cal characteristics of phenolic compounds, it is even more important to
provide protective mechanisms that can maintain the biological acti-
vities of the phenolic compounds until the time of targeting to the
organism. To reduce the environmental sensitivity and improve the
bioavailability of phenolic compounds, various microencapsulation
strategies are introduced.
3. Wall materials
Spray drying has been proved to be an effective method for the dry-
ing and microencapsulation of phenolic compounds. For spray-drying
microencapsulation, the selection of appropriate wall materials is the
crucial step. Wall material is an important part of the microencapsu-
lation and the characteristics of wall materials, including molecular
structure, wall material film properties, emulsification stability and
rheological properties, are decisive factors affecting the functional prop-
erties and process conditions of the microencapsulation, such as the size
of the emulsion droplets, the water content, yield, efficiency, apparent
morphology, particle size distribution, bulk density and other physical
and chemical properties. Among them, the rheological properties of
the feed liquid formed by the wall materials can explain and predict
the texture changes that occur during processing, and directly affect
the effect of microencapsulation (stability, dispersibility, release charac-
teristics, embedding rate and other physical and chemical properties).
The level of microencapsulation yield and efficiency are important
references to measure whether the wall materials are suitable for mi-
croencapsulation, which can reflect the embedding degree of the core
material and the quality of the product. In order to achieve the best mi-
croencapsulation performance, optimal wall materials should be se-
lected based on specific needs of the natural bioactive ingredients,
such as sensory properties, physicochemical stability, bioactive reten-
tion, loading and release [1]. Overall, ideal wall materials are supposed
to have high solubility, low hygroscopicity, effective emulsification,
flavour masking capability, well film formation, and low economic
Table 2
A brief overview of different types of wall systems.
Wall systems Single type
Carbohydrates
Microencapsulation polycondensed reaction, Maillard reaction
mechanisms [26]
Advantages low price, low viscosity, good solubility, good
oxidation resistance
Drawbacks poor film formation, low emulsifying ability, high
porosity
Examples starch and their derivatives (maltodextrins),
modified starches (octenylsuccinate starch),
cellulose and their derivatives (HPMC), plant
exudates and extracts [27]
Powder Technology 394 (2021) 562–574
costs. Meanwhile the concentrated solutions must have relatively low
viscosity for atomization, and should be able to protect the core material
from its deterioration.
Generally, the microencapsulation wall systems can be divided into
two categories: single type wall material (carbohydrates, proteins or
hydrophilic gums) and mixed type wall materials. The microencapsula-
tion mechanisms behind the formation of wall/core structure are dif-
ferent according to the classification of wall materials as well as the
core components. Dense matrixes of carbohydrates can be formed by
Maillard reaction and polycondensation reaction. Proteins can be in-
terconnected by hydrophobic interaction and covalent disulphide
crosslinking. Hydrophilic gums can be held together through hydropho-
bic interaction or polycondensed interaction. The brief summary of each
type of wall systems is listed in Table 2 below.
Regarding wall materials, carbohydrates such as starch, syrup,
maltodextrin, chitosan and small molecule sugars, are the most popular
candidates for water soluble core materials because of the high reten-
tion and low viscosity at high core materials content. As the most com-
mon type of carbohydrates, maltodextrin (MD) is a starch-based
material obtained from acidic or enzymatic hydrolysis [33] with differ-
ent DE values (DE: the number of glucose residues contained in the dex-
trin molecule). Octenyl succinate starch is the most widely used
modified starch which introduces hydrophobic side chains (octenyl)
on the basis of starch chains, and thus has amphiphilic properties with
low solution viscosity and low moisture absorption [34]. By contrast,
small molecular sugars such as sucrose, glucose and trehalose are gener-
ally not suitable to be used alone as wall materials because they are
prone to agglomeration, and are subject to caramelization during
spray drying. Carbohydrates are not desirable wall material for hydro-
phobic core materials due to the high porosity and low emulsifying ca-
pacity, which can easily to lead to low microencapsulation yield and low
glass transition temperature. Generally, it needs to be modified by some
chemical modification, or combined with other wall materials (proteins
or water-soluble gums).
In turn, the amphoteric properties of proteins make them possible
for the well wrapping of hydrophobic core materials, especially for the
microencapsulation of perfumes [35]. The most commonly used pro-
teins include whey protein, casein, gelatin etc. Gelatin is a collagen de-
rived from animal connective or epidermal tissues, which has good
emulsification, film-forming, water-solubility, wide sources, and low
price. Whey protein is mainly divided into two categories: whey protein
concentrate (WPC) and whey protein isolate (WPI). The protein content
of WPI is more than 90% while that of WPC is around 30–80%, therefore
WPI is more suitable as an emulsifier [36]. Faldt et al. [37] pointed out
that sodium caseinate is a better wall material than whey protein be-
cause it has better heat resistance. In general, different types of proteins
may show large performance differences during microencapsulation
Mixed type
Proteins Hydrophilic gums Two or more mixed
hydrophobic interaction, hydrophobic interaction and covalent crosslinking，
covalent disulphide polycondensed interaction hydrophobic interaction and
crosslinking chelation
good solubility and good film-forming and easy tunable properties to have
emulsification, low costs emulsifying properties, good good stability and encapsulation
solubility efficiency
sensitive to environment, sensitive to oxygen and not all combinations meet the
unstable quality of products environment, low stability properties required
due to batch to batch
variations
vegetable plant extracts (gum arabic), alginate-chitosan [30], whey
proteins (soy proteins), microbial products (xanthan protein-maltodextrin [31] waxy
animal protein (dairy gum) seaweed extract maize starch-octenyl succinic
proteins, gelatin, sodium (alginate) [29] anhydride [32]
caseinate) [28]
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W. Lu, X. Yang, J. Shen et al.
applications, and most proteins are sensitive to the external factors such
as temperature, ionic strength or pH, which lead poor stability of encap-
sulated materials in vivo/vitro.
Hydrophilic gums are long-chain macromolecular polymers, which
can be dispersed and swelled in water, and have good film-forming
and emulsifying properties. In comparison, hydrophilic gums like pectin
are better encapsulant than proteins in terms of seldom degradation
in vivo gastrointestinal tract [38]. It was reported that pectin can be
used as wall material for controlled release, targeted delivery and pro-
tection of natural bioactive ingredients [2]. However, most reports
have focused on the using of pectin with other wall materials, usually
with proteins instead of using it alone. As a wall material, gum arabic
has outstanding emulsifying properties, but its performance is difficult
to achieve standardization because it is a natural exudate collected
from branches and stems. In addition, the unstable performance and
expensive price have limited the application of gum acacia in some
extent. In view of the shortcomings of a single gum, many researchers
employed composite wall materials to achieve functional properties
that hydrophilic gums do not have when used alone.
As we know, single type wall materials sometimes cannot satisfy the
properties required, and one alternative is the chemical modification of
existing wall materials to get ideal properties. For instance, Peng [39]
synthesized a chitosan derivative “mPEG-g-CS” as new wall material
to encapsulate seaweed oil, which greatly improved the encapsulation
efficiency. However, the development of new wall materials generally
requires high costs, and thereby another feasible and convenient
method is the incorporation of other wall materials as modifiers, i.e.
mixed type wall materials. For example, Augustin et al. [40] proposed
to use Maillard reaction products of proteins and carbohydrates at
high temperatures to improve the stability of proteins and the emulsify-
ing property of carbohydrates. The products have good antioxidant
functions and can form a stable protective shell to encapsulate easily ox-
idizable components. In short, the expansion of the performance of sin-
gle wall material is still mainly solved by the combination of different
wall materials. Usually, some emulsifiers, plasticizers, antioxidants,
etc. are also introduced to amplify the advantages of original wall mate-
rials or eliminate their own disadvantages. Considering the structural
heterogeneity of phenolic compounds, the strategies in terms of selec-
tion of wall materials for spray drying will be discussed according to
the properties of different types of phenolic compounds.
4. Selection of wall materials for spray-drying encapsulation of
phenolic compounds
The encapsulation of phenolic compounds by spray-drying involves
(i) preparation of the feed solution, (ii) atomization, and (iii) dehydra-
tion. Normally, for the preparation of the feed solution, wall materials
are dissolved in solutions with stirring and core materials are added to
the solutions with or without the addition of an emulsifier, depending
on the water solubility of core material and emulsifying properties of
the wall materials. For hydrophilic phenolic compounds, there is no
need to apply emulsifiers during their spray drying. And for hydropho-
bic phenolic compounds, emulsion droplets can be formed by adding
wall materials with good emulsifying property or adding emulsifiers
to wall materials with poor emulsifying property. In this section, the
chemical structures, physicochemical properties, and pharmacological
benefits of 5 typical phenolic compounds are summarized. And the rep-
resentative wall materials used for spray drying microencapsulation of
these compounds are presented in the following tables (Tables 3–7), in-
dicating the important issues in terms of the selection of wall materials.
4.1. Anthocyanins
Anthocyanins, generally accepted as the largest and most significant
group of water-soluble natural pigments, are naturally occurring
phenolic compounds responsible for the bright blue, red, or purple
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Powder Technology 394 (2021) 562–574
pigments in fruits, flowers and vegetables [41]. In 1940s, Jack, a French
doctor, firstly discovered that anthocyanins were present in the coating
of peanuts [42]. After that, more than 500 species of anthocyanins were
reported, mainly existed in 27 plants [43]. The most abundant anthocy-
anins in plants are as follows: cyanidin (50%), pelargonidin (12%),
delphinidin (12%), peonidin (12%), petunidin(7%), and malvidin(7%)
[44]. As so far, structures of 22 species of anthocyanins have been iden-
tified, and more than 90% of the anthocyanins isolated are based on 6
anthocyanins (pelargonidin, cyanidin, peonidin, delphinidin, petunidin,
and malvidin) [45]. In the natural state, there are few free anthocyanins,
and most of them mainly exist in the form of water-soluble glycosides
and acyl-glycosides [46].
Anthocyanins are well known as natural colorant and additives.
Recently, the research interest of anthocyanins in nutraceutical diet
and disease prevention has increased because of their antioxidant capa-
bility. Numerous studies show that anthocyanins are capable of reduc-
ing diabetic and obesity, and can act as neuroprotective agents [47]. In
addition, anthocyanins can promote recovery of vision complications,
prevent some types of cell damage, as well as inhibit cancer growth [48].
However, anthocyanins are unstable and susceptible to degradation,
which is the main cause of low bioavailability. The particular chemical
structure of anthocyanins is easily affected by pH, light, temperature,
and oxygen [49,50]. For example, anthocyanidins appears as a red pig-
ment or a blue pigment in acidic or alkaline conditions, respectively
[51]. In general, anthocyanins are stable at pH < 3.5, like stomach con-
ditions, but they degrade at high pH values (pH > 7), like intestinal
tract conditions [52]. Microencapsulation by spray-drying is capable to
efficiently stabilize, protect, and preserve anthocyanins against nutri-
tional and health losses. In this sense, spray-drying encapsulation is
not only necessary but also convenient to preserve anthocyanins' origi-
nal color and potential bioavailability.
A number of approved wall materials are available for spray drying
microencapsulation of anthocyanins, but anthocyanidin retentions
would inevitably be cut back at outlet temperatures above 90 °C. [80]
MD was the most commonly used single carrier agent for anthocyanidin
due to good heat resistance and few browning reactions occurs. As
shown in Table 3, some comparisons under the same conditions, MD
was an excellent choice in retaining maximum anthocyanidin and its
encapsulation efficiency compared to most of the other single wall ma-
terials (e.g.GA, TS, [57] WPI and PPI [63]). The amount of MD (3 g–6 g)
for microencapsulation only minorly influenced the value of
anthocyanidin retention, but it largely influenced the stability of
anthocyanidin [53]. Although emulsifiers may not be essential during
spray drying for hydrophilic anthocyanidin, the poor emulsifying per-
formance of MD would result in less stable encapsulation system. An
improved encapsulation strategy is the combination of MD with other
wall materials, such as MD + GA [58–61], as the most common combi-
nation, showed better encapsulation properties than MD due to better
emulsification. Meanwhile, GA can be incorporated when the final
products of anthocyanins demand slow release [61]. There are of course
other satisfactory wall materials, e.g. OSA gave good storage stability
[69], HDPAF provided high anthocyanins retention and protection [74]
and AF showed excellent antioxidant activity [75]. Additionally, it is
promising to reduce the degradation of anthocyanin by applying
copigmentation and spray-drying microencapsulation in tandem. [60]
These strategies about the selection of wall materials can be potentially
employed for spray drying encapsulation of other hydrophilic core ma-
terials.
4.2. Gallic acid
Water-soluble gallic acid (3, 4, 5-trihydroxybenzoic acid) is consid-
ered as one of the major phenolic acids, in the form of ester compounds
or free acids [81]. Gallic acid is a yellowish white crystalline phenolic
compound [82], emerged as an efficient apoptosis inducing agent and
seems more stable than other phenolic compounds [83,84]. The results
W. Lu, X. Yang, J. Shen et al. Powder Technology 394 (2021) 562–574

Table 3
Summary of representative studies on spray-drying encapsulation of anthocyanins.

Source Wall Materials Formulation Conditions Spray-drying Conditions Main Results Reference

Inlet temp Outlet temp

(°C) (°C)

Blackberry MD C:W = 1:3–1:6 150 90 the amount of MD showed minor effects on anthocyanin [53]
retention (78–84%)
Blackberry MD DE10 C:W = 1:1, 170 105 MD was efficient in reducing the degradation (from 77.7% to [54]
C was 500 mg/mL 36.3%) at low pH 3–5
Red wine MD DE10 C = 2.27% (w/v), 135–170 75–79.8 the retention of anthocyanins>83% [55]
W = 13.5% (w/v)
Sour cherry MD DE4–7, C:W = 1:1, 1:2, 1:3 200 99–102 MD DE13–17 displayed the best performance at C:W = 1:3 [56]
juice MD DE with the retention of anthocyanins>89%
13–17, GA
Black carrot MD, GA, NR 150 76 MD performed the highest EE (87%), and better than GA [57]
juice TS (82%), TS (64%)
Barberry MD, C:W = 1:4 150 108 MD + GA showed the highest stability and EE (93%) [58]
MD + GA,MD + GE
Palm fruit MD + GA= C:W = 2:3, 126 89 a great retention (150 mg/100 g) of anthocyanidin and EE [59]
pulp 1:1 anthocyanin (83%)
content = 181 mg/100 g
Black rice MD, C:W = 1:4 150 NR MD + GA resulted the ingredient most stable to the storage [60]
GA, and thermal protection
MD + GA=
1:1
Red-fleshed MD + GA= C:W = 3:10 150 100 high EE (93.84–96.85%) [61]
apple 2:3
Jaboticaba MD, W = 30% (w/v), 140,160,180 NR MD + GA had the highest anthocyanins retention (100.23%) [62]
peel MD + GA,MD + CP total solid= and antioxidant activity at 160 °C
17.4%
Tamarillo MD， C:W = 1:4, 150 70 GA had the highest EE (83.1%), while OSA achieved the [63]
juice GA, W = 20% w/w juice greatest storage stability
RMD,
OSA
Barberry MD + GA + GE C:W = 3:25, 150 100 C:W = 1:4 resulted in the highest EE (96.2%) and storage [64]
1:4, 7:20, 1:2 stability
Choisy fruits MD + GA + TP anthocyanin 150 100 high antioxidant activity (69.90%) and anthocyanin content [65]
content = 325 mg/100 g (93%)
Acerola MD + CTG C:W = 1:2–1:5 170–200 NR maximum degrees of retention (>95%) at inlet temperature [66]
pomace of 170 °C, C:W = 1:5
Black MD + FG + MCC total solid= 120 78 anthocyanin retention of 82.72% [67]
raspberry 10.0%
Chokeberry MD + GA, C:W = 1:3 140 NR MD + GA had the highest moisture content and the biggest [68]
MD + IN, particles, MD + GG had the highest EE (93%)
MD + PEC,
MD + GG,
MD + β-glucan
Rape marc MD, C:W = 1:0.3–1:2, 140 NR MD particles with C:W = 1:1 showed best stability and [69]
phenolics WPI, total solid= drying yield (75.6%)
PPI 4.6–10.6%
Jussara pulp GA + WPC + modified C:W = 1:1 150 90–98 anthocyanin retention of 55.12–95.05% [70]
starch
Blueberry MD, GA, WPC and their C:W = 1:1, 180 78.5 MD had the highest EE (95.79%), MD + WPC had the highest [71]
combinations W = 10% (w/v) retention (115%)
Black rice MD, GA, WPI and their W = 15% (w/v) 180 70–80 MD exhibited the highest retention [72]
combinations (88%), WPI exhibited the highest antioxidant activity
Berries and AF, W = 0.5% (w/v) 180 80 MD + GA exhibited the highest EE (84.09%) [73]
roselle WPI,
MD + GA
Pitanga juice MD, C:W = 1:4, 1:5, 1:6 110,120,140 80 ~ 90 HDPAF with C:W= [74]
HPAF, 1:6 had the highest retention (61%) and protection
HDPAF
Blue corn AF W = 6%, 8%, 10%, 12% 150 85 6% (w/v) AF had highest retention (73%) and antioxidant [75]
(w/v) activity (42%)
Blackberry AF W = 50%, 75%, 100% 80 60 C = 50%(w/v)had the highest retention (79%) [76]
(w/v)
Saffron β-glucan, β-CD C:W = 1:5 130 80 β-glucan had better EE (63%) than β-CD (45%), and β-CD [77]
could improve stability during GI tract conditions
Maque juice SC, C:W = 1:0.5–1:4 150–190 NR when C:W = 1:4 IN had the highest EE (65.6–78.6%) at [78]
IN 162 °C, while SC only had 51.2%
Grape GA, PD, NR 140 NR GA + PD had the highest retention (94.3%) and antioxidant [79]
PHGG and their activity
combinations

NR: Not reported; C: core material; W: wall material; EE: encapsulation efficiency; Cmax: the average peak concentration; MD: maltodextrin; RMD: resistant maltodextrin; GA: gum arabic;
CP: Capsul™; TS: tapioca starch; GE: gelatin; OSA: octenyl succinic anhydride modified starch; TP: tricalcium phosphate; CTG: cashew tree gum; CD: b-cyclodextrin; FG: fenugreek gum;
MCC: microcrystalline cellulose; IN: inulin; PEC: pectin; GG: guar gum; AF: agave fructan; HPAF: high performance agave fructans；HDPAF: high degree of polymerisation agave fructans;
WPI: whey protein isolate; PPI: pea protein isolate; WPC: whey protein concentrates; SC: sodium caseinate; PHGG: partially hydrolyzed guar gum; PD: polydextrose.

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of clinical studies have reported gallic acid is a non-toxic secondary me-
tabolite from plants and fungi up to the level of 5000 mg/kg body
weight, when given orally [85]. And its distribution covers different
families of vegetables, tea, Chinese herbology, as well as in fungi of the
genus [86]. Owing to the scavenging ability and antioxidant nature
towards free radicals, gallic acid can be extensively applied in foods
as additives and preservatives [87], and also in charge of many other
important pharmacological activities, such as the prevention of
neurodegenerative diseases, oxidative DNA damage, diabetes, myocar-
dium infarction and obesity, gastroprotective and neuroprotective
effects [88].
As mentioned earlier, gallic acid has better stability than other phe-
nolic compounds under acidic conditions, strong light conditions and
even high temperature. Research showed that no significant effect of
storage temperature (4, 25 and 40 °C) on gallic acid retention was de-
tected during the 50-day storage period and the degradation during
storage followed the first-order kinetics [89], as a proof that gallic acid
is not a phenolic compound that exhibits instability under normal cir-
cumstances. Gallic acid is often in the bound form and only be freed or
hydrolyzed upon acid or alkaline hydrolysis, or by enzymes [90]. But
as a phenol or organic acid, gallic acid has the property that it is unstable
under alkaline and strong oxidation conditions [91]. From the absorp-
tion metabolism point of view, gallic acid is easily absorbed in the
digestive tract and has a strong affinity to heart, kidneys and liver. For-
tunately, some studies dealing with the biological effects of gallic acid
have reported that although gallic acid is extensively metabolized
after absorption, its metabolites can still exert a significant antioxidant
action in vivo [83]. Thus, the main limitation should be overcame is to
increase the stability in alkaline and oxidation resistance of gallic acid
during the employment of spray drying as the encapsulation method.
Similar to anthocyanins, MD is also the main wall material for water-
soluble gallic acid (Table 4). The main difference is that, as expected, the
temperature requirements for spray-drying gallic acid are not as strict
as other phenolic compounds, the optimum inlet temperatures were
mainly concentrated at 170–200 °C. Fairly good encapsulation effect
could be achieved for most wall materials except for potato starch
[97], with a lower encapsulation efficiency (<85%) than the other car-
bohydrates (MD [93], HPβCD [99] and IN [100]). Moreover, Moreno
[95] found that both WPI and PPI show satisfactory performance in
terms of the retention of total phenolic content and antioxidant activity
at low wall/core ratio of 0.1:1, which would provide ideas to increase
the concentration of phenolic compounds in the final product. Gimbun
[96] et al. further verified that the gallic acid encapsulated with WPI-MD
(1:9) yielded the best retention compared to that encapsulated by WPI
or MD alone, and the finding indicates that protein acts as a protective
layer to enhance the stability of gallic acid during spray drying. It is
worth mentioned that some studies have reported that covering lipo-
somes with wall materials is another effective way to improve the struc-
ture stability of encapsulated products from negative environment
conditions. [19,93,94] But in summary, there are few studies on the
microencapsulation of gallic acid, and the phenomenon is likely related
to the good stability of gallic acid and thereby has not much value for
improvement.
4.3. Catechins
Catechins are flavanol compounds extracted from plants, particu-
larly from tea [101,102], which accounts for more than 80% of the tea
polyphenol content in tea [103]. Catechins can be divided into two
types: ester type and non-ester type, and non-ester type catechin
displayed relatively weaker astringency than ester catechins [104].
There are more than 30 kinds of tea catechins reported, mainly includes
catechin (C), epicatechin (EC), epicatechin gallate (ECG), Epigallocate-
chin (EGC), Catechin Gallate (CG), Epigallocatechin Gallate (EGCG),
Gallocatechin Gallate (GCG), Gallocatechin (GC) [105]. EGCG is the
most abundant biological active ingredient of green tea extract, ac-
counting for 50–80% of the catechin content [106].
Catechins have been recognized as the ideal anticancer substance
extracted from natural plants and non-toxic and natural food additive
to human body [107]. A large number of clinical evidences proved the
relationship between consumption of catechin-rich foods and preven-
tion of several human diseases, including hypertension, cardiovascular,
cancer [108–110], and influenza virus [111]. Studies shown that the
ability of EGCG to resistant oxidants and radiation is 200 times of vita-
min E [112]. Moreover, the effect of catechins on reducing endothelial
dysfunction and inflammation has been confirmed in hypertensive
subjects [113].
However, the practical applications of catechins are restricted
because of its sensitivity to high temperature and pH values. It would
undergo epimerization under high temperature or alkaline pH which
further results in deterioration of the catechin activity [114]. A major
drawback of catechins is the metabolism in the gastrointestinal tract
make it a predicament to develop their potential in food matrices, and
its poor water solubility, astringency and bitterness are the other factors

Table 4
Summary of representative studies on spray-drying encapsulation of gallic acid.

Source Wall Formulation Spray-drying Main Results Reference

materials Conditions Conditions

Inlet temp Outlet temp

(°C) (°C)

Sucrose MD + GA W = 10%, 20%, 30% 100 NR the optimum spray-drying conditions [92]
were achieved when C = 10–20%
Gallic acid APIs MD coated liposome C:W = 1:4, 170 75 had high EE (97.1%) [93]
total content of C = 0.5 g
Cacao CS coated liposome NR 170 75–80 the EE was increased (87.5%) compared to [94]
without liposome encapsulation (73.6%)
Grape MD, C:W = 1:0.1 140 81 though all the W showed high recovery (>87%), [95]
WPI, WPI and PPI showed better total phenolic and
PPI cellular antioxidant activity than MD
Phyllanthus niruri MD, WPI:MD =1:9, 180 NR MD+ WPI yielded the best retention 88.93% [96]
WPI, total solid=
MD + WPI 20%
Gallic acid APIs (98%) potato starch C:W = 1:2 160 75 the EE was 70–84% [97]
Gallic acid APIs HPβCD C:W = 1:1 120 70 high EE (>90%) [98]
Gallic acid APIs (99%) HPβCD C:W = 1:1 145 90 the EE was 89.22% [99]
Green tea IN C:W = 1:25, 168 70 high EE (95.9–98.6%), but could not control [100]
total content of C = 0.5 g gallic acid release

CS: chitosan.

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cannot be ignored [115]. Thus, it is necessary to explore methods to im-
prove the stability and solubility of catechins by technical microencap-
sulation, such as spray drying, to ensure their physiological activities
and bioavailability.
As shown in Table 5, the commonly used wall material MD showed
no competitiveness compares to GA or other mixed wall materials in
terms of better process efficiency because of the hydrophobic nature
of catechins, reflected not only in encapsulation efficiency but also re-
tention rate and antioxidant activity. According to the data above, wall
materials with good emulsifying properties, including hydrophilic
gums (GA [117–119]) and proteins (GE [120] and WPI [124]), are
more suitable for the microencapsulation of catechins than carbohy-
drates (MD, CH and IN) with low emulsifying ability. Thereby we spec-
ulate that for catechins, its hydrophobicity is a main limiting factor that
should be considered preferentially. Secolin [122] further verified that
combining HPSC with carbohydrates in the encapsulation system can
also improve the oxidation resistance and stability of catechins, which
may be attributable to lipid materials can protect antioxidant polyphe-
nols from environment or other physicochemical factors. Taking into ac-
count that drying temperature is a another key element to influence tea
catechin stability during spray drying, encapsulation of catechin at low-
temperature of 130 °C using 12 different wall materials is compared di-
rectly by Belščak [123], and the result showed that WPI and IN are able
to preserve various inherent biological activities of catechins at low
temperature. To a greater extend, wall materials that can help core ma-
terials resist the severe environmental conditions such as high temper-
ature or high pH can become the direction of future research. Different
opinions were put forward by Zokti [118], low-temperature spray dry-
ing was found not to be essential for catechins' retention, and it may
be a better approach to store catechins powder at temperatures below
25 °C for increased shelf-life. However, there are few studies about the
effects of wall materials on the gastrointestinal metabolism of catechin,
which is detrimental to the using of catechins in food or pharmaceutical
products.
4.4. Resveratrol
Resveratrol (3,5,4′-trihydroxystilbene), a natural non-flavonoid
polyphenolic compound of Stilbenes，has a carbon‑carbon double
bond in the molecular structure [125]. There are both trans and cis
forms in resveratrol, and the trans-structured resveratrol has stronger
physiological activity than the cis-structure [126]. Resveratrol can be
found in many plants, such as grapes, peanuts and berries, which has
been used in traditional medicine as well as in modern health care
products [127]. In clinical studies, resveratrol has shown a variety of
pharmacological activities, such as anti-oxidation, anti-inflammatory,
cardiovascular protection, neuroprotection and anti-aging [128]. At
the same time, resveratrol also shows anti-cancer activity against
some tumor cells, such as esophageal cancer, prostate cancer, breast
cancer, skin cancer and colon cancer [129–131].
Despite the large amount of data concerning on resveratrol, very lit-
tle is known about the bioactive forms of the resveratrol metabolites
in vivo. The reason is that the solubility of resveratrol is poor
(0.02–0.03 mg/mL) [132] and the bioavailability is less than 1% due to
rapid first pass metabolism. There is accumulating evidence suggesting
that resveratrol is rapidly metabolized in the human liver and intestine
[133], which affects its nutritional value and bioavailability. However,
many studies focus on improving the solubility instead of the question
of their achievable concentrations in the circulation after ingestion as
well as the possibility of metabolism. In fact, several studies have
shown that even if the solubility of resveratrol increases up to 59,500
times, its bioavailability is not significantly improved [134]. Therefore,
the metabolism and dosage of resveratrol cannot be ignored during
the processing via spray drying technology.
Comparing the phenolic compounds mentioned above, it should be
noted that the main drawback of resveratrol is its photosensitive and li-
pophilic properties. Table 6 showed that the incorporation of emulsifier
or biopolymers with emulsifying ability, especially protein (SC, WPC), is
required for wall materials. The assessment of SC as the most common
wall materials for resveratrol showed that SC-based microcapsules pro-
vided high bioavailability, solubility [137], digestive stability, [138] en-
capsulation efficiencies and resveratrol retention [139]. Another
interesting finding was that the encapsulation of resveratrol with SC sig-
nificantly increased the taste detection threshold compared to
unencapsulated-resveratrol [136], implying that SC may provide the
food industry a way to add the bioactive ingredients with astringency
and bitterness into a wide range of food products without negatively af-
fecting sensory. Beyond all doubt, there were almost no study using car-
bohydrates alone as wall material due to the hydrophobicity of
resveratrol. Some uncommon wall materials (DPPC+HA [141], SRAS
[143]) was also employed to encapsulate resveratrol instead of carbohy-
drates providing high encapsulation efficiency (>95%). Oddly, there
were no reports about the use of hydrophilic gums as wall material for
resveratrol, even though hydrophilic gums have good emulsification

Table 5
Summary of representative studies on spray-drying encapsulation of catechins.

Source Wall materials Formulation Spray-drying Conditions Main Results Reference

Conditions
Inlet temp Outlet temp
(°C) (°C)

Green tea MD, CD, C:W = 1:1, 120 60 MD encapsulates had the highest EE (69%), while MD+ [116]
MD + CD total solid= CD had the highest antioxidant activity
0.83 g
Fermented tea leaf MD, C:W = 1:10, 150 90 GA had the highest EE (98%), and MD was 89%, [117]
GA, total solid= modified starch was 81%
modified starch 4.53%
Green tea MD, GA, C:W = 5%:95% (w/w) 150 NR GA had the highest EE (88.04%), MD+ GA + CTS [118]
CS and their combinations had the highest antioxidant capacity (38.05%)
Green tea MD + GA C:W = 5 wt.%:95 wt. 150 50 EE was 96 ± 3%, with mean average diameters [119]
% of 40–400 nm
Purified EGCG CS, GE C:W = 1:9 90 44–50 GE achieved higher EE (95 ± 6%) than CH (82 ± 9%) [120]
Purified IN C:W = 1:40 145 NR had low EE (69.9%) [121]
epicatechin
Green tea HSPC+CS NR 100–150 NR the highest EE achieved at 120 °C from 31.0 ± 15.5% [122]
to 74.3 ± 6.4%
Green tea WPI, PPI, IN, GA, G, PEC total solid = 1.5% 130 56 IN provided highest EE (82.16 ± 4%) [123]
Cocoa WPI C:W = 1:3 180 88 catechins retention of 70.66 ± 1.5% [124]

HPSC: hydrogenated soy phosphatidylcholine.

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Table 6
Summary of representative studies on spray-drying encapsulation of resveratrol.

Source Wall Formulation Conditions Spray-drying Main Results Reference

materials Conditions

Inlet temp Outlet temp

(°C) (°C)

Peanut sprout MD，WPC C = 1 mg/mL, W = 30% (w/v) 170 70 WPC had higher resveratrol retention (89%) [135]
than MD (77%) and exhibited higher stability
during storage
Resveratrol APIs SC C:W = 4.8%:95.2% (w/w) 160 90 successfully masked taste or other sensory [136]
characteristics of the compound
Cacao SC C:W = 26 mg:660 mg 90 45–50 the bioavailability was 26.5%, 10 times higher [137]
than before encapsulation
Purified SC, W = 4 g, total solids = 4.8% 160 90 SC provided a higher digestive stability and [138]
trans-resveratrol WPC bioaccessibility (86–81%) compared to
WPC (71–68%)
Resveratrol APIs (98%) SC + MD total solid concentration = 30 g/100 g 180 93.3 high resveratrol retention (80–100%) and [139]
+ DGS EE (>97%)
Resveratrol APIs (>98%) SC + G + DGS SC:G:DGS = 1:1:1, 180 80 high EE (98%) and stability, after [140]
C = 25 mg 18 months at 25 °C
storage there was 81–100% remaining
Resveratrol APIs DPPC+HA DPPC:HA = 4:1，W = 1 g 180 NR high EE (≥97%) [141]
Resveratrol APIs (98%) HPMC C:W = 9.6 wt%:90.4 wt% 105 50–60 resveratrol in encapsulation could retain [142]
86%, while raw
resveratrol only remained 20%
Resveratrol APIs (98%) SRAS+Tween80 SRAS = 2 g, Tween80= 140 65 high EE (95.4%), and the stability, the [143]
0.5 g, C = 0.132 g antioxidant activity,
and bioavailability were increased

G: glucose; DGS: dried glucose syrup; DPPC: dipalmitoyl phosphatidylcholine HA: hyaluronic acid; SRAS: Shellac resin ammonium salts.

properties. We speculate that hydrophilic gums with instability and ox-
idative properties may not be suitable for encapsulating equally sensi-
tive resveratrol, but there are no related reports as the basis for this
hypothesis. Regrettably, degradation and metabolism in the gastroin-
testinal tract is closely related to the low bioavailability of resveratrol,
but almost all encapsulation strategies had not faced this issue.
4.5. Curcumin
Curcumin has been widely acknowledged as dietary supplement in
the world, which is an herbal low-molecular-weight polyphenolic
compound mainly derived from traditional Chinese herbal medicines
such as turmeric [144]. Its pharmacological effects have gained signi-
ficant research attention, especially in the areas of anti-depressant,
anti-hyperlipidemia, anti-diabetic, anti-inflammatory and anti-viral
[145,146]. In particular, various clinic studies have demonstrated
that curcumin is safe and could be tolerated even at dosages as high as
8 g per day [147].
In spite of its appreciated pharmacological effects, curcumin is a
highly lipophilic compound and has poor solubility in water, which
has been argued as a potential reason limiting its absorption in the
human body [148]. On the other hand, instability at physiological pH,
the relatively high rate of metabolic elimination from the intestinal
and liver enzyme systems, and inactivity of the metabolic end-
products results in a low oral bioavailability of curcumin [149]. And
the poor bioavailability and high dosage of curcumin limits complete
translation of in vitro benefits into clinical conditions. Hitherto, some
drug delivery strategies have attempted to encapsulate curcumin
using delivery systems, such as spray drying of solid dispersions,
which has been regarded as a promising strategy to enhance the
systemic bioavailability of curcumin.
Different wall materials were employed for spray drying encapsula-
tion of curcumin as summarized in Table 7. It can be seen that, the
choice of wall materials for curcumin is more extensive than the four
previously mentioned phenolic compounds. The photochemical stabil-
ity of curcumin encapsulated with CH-Tween 20 has been evaluated
by O'Toole et al. [150], they concluded that the incorporation of Tween
20 not only improved the stability of curcumin, but also prevented its
degradation. Similar observation using Tween 80 was also reported by
Hu et al. [153] Analogously, MC, [154] SC, [155] WPI [156] and GA
[158] showed good performance in terms of encapsulation efficiency,
retention rate or antioxidant activity, which proved to be the ideal
wall material for curcumin. Oppositely, β-CD has been considered un-
suitable as a wall material for polyphenols due to its low product recov-
ery and encapsulation efficiency. [162] In this line, some unusual wall
materials, GLC-Aerosil® [152], Eudragit® EPO [157] and WPI [159],
can result in remarkable fold enhancement of curcumin solubility.
What needs to be added is that, assembled wall materials by interaction
between OSA and GA [161], could provide the encapsulated curcumin
good acid fastness stability and light stability. The last point is that
study showed sodium octenyl succinate modified starch (SOSMS) can
improve the stability of curcumin against alkaline condition [165].
These studies are helpful to provide a strategy for enhancing acid-base
stability and can be extended to other active substances.
5. Discussion and conclusion
The microencapsulation afforded to phenolic compounds during
spray drying is reviewed, and it is obvious that the choice of suitable
wall material is an extremely important first step. In a nutshell, to
achieve the best microencapsulation, appropriate wall material should
be selected and relied on the physical-chemical properties of core mate-
rial and the application intended for the product powder. The overview
of the microencapsulation strategy of phenolic compounds was shown
in Fig. 1.
Firstly, solubility is the basic property of active ingredients and is
also the primary consideration for choosing wall materials. There is no
requirement to apply emulsifiers during selecting wall materials for hy-
drophilic phenolic compounds (anthocyanidins and gallic acid), so car-
bohydrates are the most popular candidates of wall materials. One of
the most commonly used carbohydrates is MD, which is cheap and
useful for enhancing the encapsulation efficiency of hydrophilic core
materials. Oppositely, for hydrophobic phenolic compounds (catechins,
curcumin and resveratrol), wall materials composed of carbohydrates
may has large pores or non-emulsifying capability and can't meet the
stability requirements of encapsulation system, thus proteins and
hydrophilic gums are preferred over carbohydrates as wall materials be-
cause of their hydrophobic cavities. Another idea is that emulsifiers or

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Table 7
Summary of representative studies on spray-drying encapsulation of curcumin.

Source Wall materials Formulation Conditions Spray-drying Main Results Reference

Conditions

Inlet temp Outlet temp

(°C) (°C)

Rhizome CS + Tween 20 W = 0.1% (w/v), 120 NR 12.7-fold increase of curcumin solubility, and curcumin [150]
curcuma C = 50 mg/100 ml can be released completely from the particles over a 2 h period
Turmeric GA + COL =1:14 C:W = 15 g:30 g 170 NR low EE (42.8–56.2%), yield values:88.9–94.7%, and [151]
rhizomes higher GA led to lower yields
Curcumin APIs Gelucire® C:W = 1:1, NR 40 a remarkable 3600-fold increase of curcumin solubility in water [152]
+ Aerosil® total solids=
7.5%
Curcumin APIs Tween 80 C = 20 g, W = 6.25% 170 90 bioavailability was enhanced about 3.2-fold, Cmax from [153]
3.64 mg/L to 27.52 mg/L
Curcumin APIs MC total solids= 180 90 high curcumin retention (97%) and high antioxidant [154]
(66%) 15.5% activity (88%)
Curcumin APIs SC C = 0.05% (w/v), 105 66 when W = 5%(w/v) had highest EE (91%) [155]
(95%) W = 0.1%–10% (w/v)
Curcumin APIs SC C:W = 1:4, 105 68 40-fold increase of curcumin solubility, and EE was 83.1% [156]
(> 90%) C=1g
Curcumin APIs Eudragit® EPO C:W = 1:1 56 42 2014-fold increase of curcumin solubility (pH 1.2), [157]
from 0.02% to 40.29%
Curcumin APIs GA C = 0.1 mg/mL, W = 20% 150 88 a product yield was 44–52%, EE was 75–85% [158]
(≥98%) (w/v)
Curcumin APIs WPI C = 25 mg, 150 110 11,355-fold increase of curcumin solubility [159]
(≥80%) W = 10 wt% (124.9 ± 4.8 mg/mL), high EE (>95%)
Curcumin APIs OSCD+MD C = 0.5 g, 180 NR the curcumin retention was significantly improved [160]
(98%) W = 20 g, (from 77.00% to 93.09%)
total solid = 11.5 g/L
Curcumin APIs OSA + GA C:W = 1:20, 1:30, 1:40 190 70 EE were significantly affected by the ratio of C:W, [161]
when C:W = 1:30 had highest EE (96.1%)
Turmeric BRF + β-CD C = 5%(w/ w), 150 80 EE was 85.55%, and showed effect on masking properties [162]
W = 20 g/L
Curcumin APIs SC + Tween 80 C:W = 1:1 100 NR when Tween 80 concentration was low, could not form a [163]
well-dispersed colloidal system lead to low EE (58–66%)
Curcumin APIs HPMC+EUD C:W = 1:3, 100 NR EE was 81.8–87%, a product yield was 49.1–52.5% [164]
(65%) C = 50 mg

COL: collagen; MC: micellar caseins; OSCD: octenylsuccinated corn dextrin; BRF: brown rice flour.

Fig. 1. The overview of the microencapsulation strategy of phenolic compounds.

570
W. Lu, X. Yang, J. Shen et al.
biopolymers with emulsifying ability (such as WPI, WPC, GA and
modified starch) may need to be added into carbohydrates, leading to
substantial improvements in solubility, retention, stability and encapsu-
lation efficiency.
Secondly, the stability under spray drying, including thermal stabil-
ity, light stability and oxidative stability, is also a factor that must be val-
ued. For encapsulation of thermally unstable core materials (catechins),
wall material (WPI, IN and GA) with good encapsulation efficiency
at low temperature or wall material (OSA-GA) that can protect core ma-
terial from degradation at high temperature are frequently used. Other-
wise, it should be produced by freeze-drying if targeted core material is
a high value compound that has a high sensitivity to high temperature.
Regarding light-sensitive core materials (curcumin and resveratrol),
mixed wall materials of OSA and GA were shown to enhance stability
of photosensitive lipophilic materials [161]. In allusion to oxygen-
labile core materials, double emulsion and hybrid wall materials with/
without crosslinkers (glutaraldehyde to chitosan, transglutaminase to
protein hydrolysate) can form a hybrid shell with compact structure
providing protection against oxidative degradation [1].
Thirdly, sensory characteristics of the encapsulated products deter-
mine whether the product can be applied to a wide range of actual in-
dustries. For example, the occurrence of astringency and bitterness of
anthocyanidin, resveratrol and catechins causing negative affect attri-
butes of the products, it would be helpful to gain a better understanding
of the sensory detection threshold of their microcapsules within differ-
ent types of wall materials. According to the obtained results of a sys-
tematic sensory investigation of 12 different wall materials designed
by Belščak [123], modified starch and IN provided powders with the
highest aroma intensity and lowest astringency, while GA, PEC, WPI
and PPI could result in severe bitterness and astringency. In addition, a
recent study thereby indicated that encapsulation with SC [136]
successfully masked an unpleasant taste of resveratrol. And we specu-
late that these wall materials can also be generalizable to the flavor
researches.
Fourthly, the controlled release of core materials at the suitable place
and the suitable time is another important issue for the selection of wall
materials and is critical to certain core materials which involves acid-
base stability in the gastrointestinal tract, which refers to release rate,
release profile and target site. For products that demand prolonged re-
lease, wall materials have strong interaction with core materials
would be preferred. On the other hand, for powdered products
demanded immediately release, it is usually easier to be achieved for
samples with large pores on the surface or weak interaction between
wall and core materials. Universally, Tween 80 [153], Eudragit® EPO
[157] and double emulsions with pH-sensitive property show quick re-
lease characteristics in the intestine. For example, curcumin encapsu-
lated in CH coated with Tween 20 showed a burst release profile, and
all loaded curcumin was released within 2 h. [150] In the same way,
wall materials covered with liposomes can provide the control of the
transport and release of core materials since the metabolism of lipo-
somes mostly occurs in the small intestine in humans [93].
In the last point, there is accumulating evidence suggesting that
some phenolic compounds (gallic acid，catechins and resveratrol)
may be degraded or deactivated in some different sections along the
gastrointestinal tract due to distinct pH and enzyme conditions. Despite
the large amount of study concerning the phenolic bioactivity, only very
little is known about the possibility of metabolism and the bioactive
properties of their metabolites after ingestion. Additionally, achievable
therapeutic dosing concentration is another limitation which causing a
majority of phenolic compounds lack of commercial availability. At
present, there exist two possible measures: 1) encapsulation of the phe-
nolic compounds using specific combinations of wall materials that
have stimuli-responsive properties to break down at specific sites; Pec-
tin is a reasonable example which seldom degrade in the upper gastro-
intestinal tract and can be act as outer layers to prevent core substances
that have acid sensitivity from being metabolized and degraded in the
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Powder Technology 394 (2021) 562–574
stomach while being destroyed in the intestine to release core sub-
stances completely. [114] Crosslinked WPI shows similar function to re-
sist digestion in the gastric fluid with pepsin; [166] 2) co-encapsulation
strategies may help to eliminate metabolic effects as much as possible.
For instance, co-encapsulation of resveratrol with piperine (a metabolic
inhibitor) significantly improved resveratrol oral bioavailability [167].
Based on the criteria and information discussed above, some encap-
sulation strategies can be employed as a guidance, but all of the factors
should be considered as an entirety for the final selection of wall mate-
rials. Overall, functional properties of microcapsule products like encap-
sulation efficiency and storage stability have been optimized so far, and
we speculate that future research directions can be carried out in the
following areas: i) to improve overall delivery efficiency of natural bio-
active ingredients by assembling of the functional wall materials and
microencapsulation strategies; ii) to enhance the understanding of the
wall-core structures and formation kinetics, as well as the influence of
the combination of different wall materials and the ratio of core to
wall on the retention and release mechanisms; iii) to design nano-
encapsulation of bioactive ingredients by spray-drying to further pro-
vide precise controlled delivery and release to improve bioavailability.
In conclusion, microencapsulation of natural bioactive ingredients still
faces with a lot of challenges and opportunities for the functional
foods industry.
Declaration of Competing Interest
The authors declare that they have no conflict of interes.
Acknowledgements
The authors would like to acknowledge financial support from Na-
tional Natural Science Foundation of China (Grant No. 81503023) , Nat-
ural Science Foundation of Hunan Province (Grant No. 2020JJ5788) and
the Fundamental Reseach Funds for the Central Universities of Central
South University (Grant No. 2021zzts0989).
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