Drying Technology

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Encapsulation of bioactive compounds through

electrospinning/electrospraying and spray drying:
A comparative assessment of food-related
applications

Christina G. Drosou, Magdalini K. Krokida & Costas G. Biliaderis

To cite this article: Christina G. Drosou, Magdalini K. Krokida & Costas G. Biliaderis (2017)
Encapsulation of bioactive compounds through electrospinning/electrospraying and spray drying:
A comparative assessment of food-related applications, Drying Technology, 35:2, 139-162, DOI:
10.1080/07373937.2016.1162797

To link to this article: http://dx.doi.org/10.1080/07373937.2016.1162797

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DRYING TECHNOLOGY
2017, VOL. 35, NO. 2, 139–162
http://dx.doi.org/10.1080/07373937.2016.1162797

REVIEW ARTICLE

Encapsulation of bioactive compounds through electrospinning/electrospraying

and spray drying: A comparative assessment of food-related applications
Christina G. Drosoua, Magdalini K. Krokidaa, and Costas G. Biliaderisb
School of Chemical Engineering, National Technical University of Athens, Athens, Greece; bLaboratory of Food Chemistry and Biochemistry,
a

Department of Food Science and Technology, School of Agriculture, Aristotle University of Thessaloniki, Thessaloniki, Greece

ABSTRACT KEYWORDS
Spray drying and electrohydrodynamic processes, namely, electrospinning and electrospraying, are Bioactives; electrospinning;
the most promising encapsulation technologies for entrapping and effectively delivering bioactive electrospraying; encapsula-
compounds. Encapsulation is used by the food industry to incorporate such compounds into tion; food application; spray
drying
different food matrices, protect them from adverse environmental conditions, and thereby increase
the product shelf life and maintain the health-promoting properties of the composite formulation.
This review provides a succinct discussion on the potential of food ingredient-based applications of
spray drying and electrohydrodynamic processes on encapsulation as well as the principles and the
parameters that affect the structure–morphology of the carrier matrix and the encapsulation
efficiency of the process.

Introduction food, enhance the solubility or dispersibility of lipophi-

lic compounds, mask off-flavors without unfavorably
Due to current consumer demand for more natural
affecting the taste, aroma, or texture as well as increase
foods with fewer synthetic additives, together with a
the stability and extend the shelf life of the product.[4]
wide range of available bioactive compounds in various
There are different methods for encapsulation of food
forms (isolates, concentrates, etc.), their incorporation
ingredients. Spray drying is one of the oldest and most
in various food systems as value-added ingredients is
commonly used encapsulation techniques used in the
a growing area of research. In this regard, the range of
food industry for several decades.[6] The process is
applications for encapsulation technologies in the food
economical and flexible, uses equipment that is readily
industry has been growing due to many advantages
available, and produces powder particles of fairly good
the encapsulation offers to the preservation of bioactive
quality. During spray drying, the active material is
components instead of their direct incorporation in a
dispersed in a carrier polymer solution which is then
food system.[1] Specifically, encapsulation is defined as
atomized into small droplets. The solvent, usually water,
a technology to “package” materials in the form of
is evaporated using a hot air current with controlled
micro and nanostructures through entrapment (physi-
temperature and relative humidity to instantaneously
cal or molecular) of one active agent (core material)
obtain a powder.[7] However, the use of relatively high
within another substance (wall material).[2,3] In the food
working temperatures during the drying process may
industry, particularly, encapsulation is used to deliver a
cause heat degradation and thus affect stability of
range of food ingredients within small capsules when
thermally labile ingredients.[8] As a result, over the last
direct addition of the food ingredient compromises
few years, electrospraying and electrospinning have
the quality of the manufactured food product.[4] The
attracted widespread interest and found applications in
main objective of encapsulation is to protect the core
the food industry for the production of micro and
material from adverse environmental conditions, such
nanosized particles and fibers, respectively. These elec-
as undesirable effects of light, moisture, and oxygen,
trohydrodynamic processes have also been used for the
thereby improving the stability of the functional
encapsulation of various food and bioactive compounds,
ingredient and at the same time promoting its con-
including pharmaceuticals.[9] Electrohydrodynamic pro-
trolled or targeted release.[5] Moreover, the use of
cesses make use of high-voltage electric fields to produce
encapsulation can augment the nutritional quality of

CONTACT Christina G. Drosou cdrosou@chemeng.ntua.gr Laboratory of Process Analysis and Design, School of Chemical Engineering, National
Technical University of Athens, 9 Iroon Polytechneiou Street, Zografou Campus, Athens 15780, Greece.
Color versions of one or more figures in the article can be found online at www.tandfonline.com/ldrt.
© 2017 Taylor & Francis
140 C. G. DROSOU ET AL.
electrically charged jets from viscoelastic polymer solu-
tions which on drying, by evaporation of the solvent,
produce ultrathin polymeric structures of varying
morphologies.[10] The most interesting advantage of
electrohydrodynamic processes is that they can achieve
high encapsulation efficiencies without application of
heat treatment. The absence of heat in any electrohydro-
dynamic process is a key advantage over spray drying
and is important for preserving the structure and efficacy
of the bioactive substances upon processing storage and
delivery.[11] However, its potential in the field of food
science is less explored thus the operating conditions
for encapsulation of food bioactives as well as the proper-
ties and efficiency of the structures obtained have to be
analyzed to improve and broaden the application range
of these emerging technologies in the food industry. As
for every encapsulation technique, there is an optimal
combination of process parameters, including polymer
solution characteristics, to obtain composite structures
with desirable characteristics and high encapsulation
efficiency. Hence, the current review aims to present
the principles and the parameters that affect the particle
or fiber morphology as well as the encapsulation
efficiency obtained from both spray drying and electro-
hydrodynamic techniques with an emphasis on food
ingredient applications. Moreover, it includes the state
of the art of encapsulation of food bioactives by using
each encapsulation method.
Principles of spray drying
Spray drying is the oldest and the most widely used
encapsulation technique in the food industry sector. It
is a flexible, continuous, and economical operation that
produces particles in the range from a few microns to tens
of microns with narrow size distribution.[7,12] Encapsula-
tion by spray drying protects, stabilizes, and enhances the
solubility and controlled release of the bioactive com-
pounds which are delivered in a powder form.[13] In
Figure 1. Schematic of emulsion preparation (A) and spray drying apparatus (B).
addition, spray drying ensures microbiological stability
of the products, reduces the storage and transport costs,
and minimizes the risk of chemical and/or biological
degradations by decreasing water content and water
activity.[7] Although spray dryers are widespread in the
food industry, there are two limitations of this technique.
Specifically, the carrier material should be film forming
and soluble in water and the active substance should be
heat resistant at the temperatures usually applied for this
drying method during the relatively short exposure to the
hot air stream.[14] Encapsulation by spray drying involves
several steps as shown in Fig. 1. First, the active substance
to be encapsulated is homogenized with the carrier
material at a given ratio in a liquid medium, usually an
aqueous phase. The mixture or emulsion that constitutes
the feed solution is then pumped into the drying chamber
through a nozzle. Upon exit from the nozzle tip, the dro-
plets are atomized and come into contact with the drying
fluid, i.e., hot gas (often air) inside the drying chamber.
Subsequently, water is evaporated by the stream of hot
air and when the droplet water content reaches a critical
value, a dry crust is formed on the droplet surface and the
wall material covers the microparticles of the active
material. If the droplet shrinks very slowly, the dry crust
can also develop at inner regions of the droplet and poss-
ibly leads to the formation of a full particle. In the case of
faster water evaporation, a crust is rapidly formed on the
surface of the droplet, decreasing subsequently the rate of
the water evaporation process. Finally, the dry microcap-
sules in the form of free-flowing powder are collected at
the bottom of the dryer or in the powder collector of
the cyclone.[14–17]
Parameters influencing particle
characteristics and encapsulation efficiency in
the spray drying process
Spray drying, being the most common method of
encapsulating food ingredients, is used for coating or

entrapping a functional component within a suitable
inert carrier matrix.[18] Actually, great interest is found
in encapsulation of flavors, lipids, phenolic compounds,
and colorants, including carotenoids. Successful encap-
sulation of functional ingredients should result in a
powder with both minimum surface oil or other
entrapped constituent and maximum retention of the
core material inside the particle’s structure.[19] Quality
of the obtained product and the powder efficiency are
dependent on the operating conditions such as inlet
and outlet air temperature, feed temperature, and flow
rate as well as on the emulsion properties such as the
nature of oil phase, types of wall materials, ratio of wall
to core ingredients in the liquid dispersion, total solids
content, viscosity of the atomizing fluid, stability, and
droplet size.[20]
Feed temperature
Initially, feed temperature is one of the main factors that
affect particle morphology and encapsulation efficiency.
In fact, feed temperature modifies the viscosity (fluidity)
of the feed, its fluidity, and its capacity to be homoge-
neously sprayed. When the feed temperature increases
to a certain level, viscosity and droplet size should
decrease but excessively high temperatures can cause
volatilization or degradation of some heat-sensitive
ingredients.[7] Shu et al.[21] who encapsulated lycopene
using a gelatin–sucrose system, reported that encapsula-
tion efficiency increased with an increasing feed tem-
perature from 35 to 55°C, whereas when the
temperature was further increased to 65°C, the encapsu-
lation efficiency decreased. Similarly, the encapsulation
efficiency of lycopene using maltodextrin as wall
material increased with an increasing feed temperature
from 20 to 45°C, whereas when the temperature
increased to 70°C, the efficiency decreased
significantly.[22] This observation may be attributed to
the effect of feed temperature on emulsion viscosity.
Brückner et al.[23] reported that the ideal feed tempera-
ture for microencapsulation of food ingredients is 40°C
due to the lower feed viscosity and the higher drying
rate, which leads to a quicker formation of the dry layer
of carrier material around the droplet. On the other
hand, a feed temperature of 60°C was found to be dis-
advantageous, because it lowers the viscosity of the car-
rier material, allowing for internal mixing inside the
particle during the drying process, thus retarding the
desired formation of a semipermeable crust around
the particle.[23] Furthermore, Yamamoto et al. investi-
gated the effect of feed temperature on encapsulation
efficiency of D-limonene using a mixture of gum arabic
and maltodextrin. The results showed that the powder
DRYING TECHNOLOGY 141
prepared at a higher temperature had higher stability
against the release and oxidation of D-limonene than
that of the powder obtained at lower temperature. The
findings may be partly attributed to an increase in shell
thickness of the particle at higher temperatures. The
thicker shell wall poses a stronger barrier against the fla-
vor release as well as to the diffusion of oxygen and
moisture from the surrounding environment.[24] On
the other hand, Paramita et al.[25] reported that the
encapsulation efficiency of D-limonene is not signifi-
cantly dependent on the feed temperature.
Inlet temperature
An appropriate adjustment of the air inlet temperature
and flow rate is important through spray drying
process.[26] Specifically, the flow of the feed material
should be adjusted so that the liquid sprayed evaporates
before it comes into contact with the walls of the drying
chamber. In a recent study, powders with higher con-
tent of bioactive compounds and higher antioxidant
activity were produced at lower inlet drying tempera-
tures and higher feed rate.[27] The influence of dryer
inlet air temperatures has received considerable
attention.[28] Generally, it is desirable as the use of a
high inlet air temperature to allow rapid formation of
a semipermeable membrane on the droplet surface but
yet not so high as to cause heat damage to the dry pro-
duct or excessive bubble growth and surface disruption,
which increases losses during drying[29] or causes the
particles to become sticky and cake.[30] For instance,
the encapsulation efficiency of lycopene using malto-
dextrin as wall material increased with an increasing
inlet air temperature from 110 to 150°C, whereas when
the temperature increased to 160°C, the efficiency
remained almost constant.[22] Similarly, increasing inlet
temperature from 170 to 210°C, the encapsulation
efficiency of lycopene increased with temperature at
first, but then decreased dramatically when temperature
reached the upper limit of 210°C.[21] In addition, micro-
encapsulation of vitamin C by spray drying, using gum
arabic as a microencapsulating agent, was studied at dif-
ferent air temperatures (140–200°C) and wall material
concentrations (10–20% aqueous solutions). The high-
est concentrations of vitamin C were obtained on higher
ranges of inlet air temperature, 152°C, and gum arabic
concentration, 18%.[31] Similarly, de Souza et al.[32]
reported that with increased temperature and lower car-
rier agent concentration (10%), there was a decrease in
anthocyanin retention due to the degradation of these
molecules. Therefore, the high air temperatures should
accompanied with high solid concentration of solution
to achieve high encapsulation efficiency and
142 C. G. DROSOU ET AL.
preservation of the bioactives. Moreover, the influence
of inlet temperatures (160–200°C) on spray drying of
mandarin oil was evaluated and an increase in inlet
air temperature favored the retention of the volatile
oil.[33] Similar behavior was observed by Botrel et al.[8]
and Fernandez et al.[34] in the microencapsulation of
rosemary essential oil and fish oil by spray drying. It is
well known that an increase in inlet air temperature
(within limits) leads to the rapid formation of a semi-
permeable membrane around the emulsion droplet,
thereby providing better retention of volatiles.[35] On
the other hand, Paramita et al.[25] reported that increasing
inlet air temperature from 120 to 150°C results in lower
flavor retention on spray-dried powder. These authors
also reported that higher inlet air temperature promoted
the vaporization of flavor during drying process.
Outlet temperature
The influence of dryer outlet air temperature on bioac-
tive retention is not well documented. Actually for a
given spray dryer system, the outlet temperature
depends on the combination of inlet temperature and
feed rate. Lower outlet temperatures are reached with
higher feed rate since the amount of liquid in contact
with the drying gas is higher and therefore higher quan-
tities of heat are involved for moisture evaporation.
Although higher temperatures promote faster evapor-
ation and a rapid crust formation, it is important to take
into consideration the temperature of degradation of the
materials to minimize losses of the bioactive
compounds.[36–38] A recent work on the encapsulation
of lemon myrtle oil reported that the outlet air tempera-
ture of the spray dryer had little effect on oil retention
but the surface oil increased significantly with the
increasing outlet air temperatures, presumably due to
the temperature-mediated enhancement of oil
diffusion.[39] Another study demonstrated that a higher
flavonoid content is obtained in the powder at an outlet
drying temperature of 100°C than at 160°C.[27] In
addition, encapsulation of bitter melon was conducted
by spray drying to optimize the inlet (125.6, 130, 140,
150, and 154.1°C) and outlet (72.9, 75, 80, 85, and
87.1°C) temperatures of the process; optimal inlet and
outlet temperatures were 140 and 80°C, respectively.[40]
Table 1 summarizes the experimental conditions (inlet
and outlet temperature) for the encapsulation of differ-
ent food ingredients by spray drying.
Core–wall material concentration
There is an optimum concentration of core material
that could be encapsulated efficiently depending on
the physicochemical properties of both wall and core
materials used in a particular spray drying process.
Higher core loads resulted in poorer retention or lower
encapsulation efficiency and a higher core material con-
tent at the surface of the powder particles.[56–58] This
trend may be attributed to greater proportions of core
materials close to the drying surface, thereby shortening
the diffusion path length at the air–particle interface.
For instance, the encapsulation efficiency of lycopene
increased with an increasing core-to-wall material ratio
from 1:19 to 1:3, whereas when the ratio increased
further to 1:1.5, the efficiency decreased. Minemoto
et al.[59] also observed that the encapsulation efficiency
of linoleic acid decreased when the weight ratio of core
to wall material increased. According to these authors,
at higher ratios, the amount of wall material is not
enough to fully cover the oil droplets and this insuf-
ficiency may result in a decrease in encapsulation
efficiency. Moreover, Soottitantawat et al.[60] reported
a significant increase in the surface oil of microencapsu-
lated L-menthol when the mass ratio of L-menthol:wall
material was increased from 1:9 to 3:7, using gum arabic
and two types of modified starch (Hi-Cap 100 and Cap-
sul) as wall materials. In most of the published works, a
typical core-to-wall material ratio of 1:4 was adopted
and identified as being optimal for various wall materi-
als, such as gum arabic and modified starches.[19,61] In
another study, the encapsulation efficiency of pepper-
mint oil decreased with an increase in the initial oil con-
centration from 70.6% for 10% oil to 57.2% for 30% oil,
using maltodextrin as wall material.[46] Similar behavior
was noted by Huynh et al.[39] and Tan et al.[57] in the
microencapsulation of lemon myrtle oil and fish oil by
spray drying. In another study, the influence of wall
material concentration on the properties of rosemary
oil microencapsulated by spray drying, with gum arabic
as carrier was investigated. The results indicated that oil
retention was affected significantly (p < 0.05) by the
wall material concentration and higher oil retention
values were observed when there was a high solid con-
tent in the liquid dispersion compared with its low solid
content counterpart.[34]
Emulsion characteristics
Another important factor in the microencapsulation of
oils is the physical stability of the emulsions from which
particles are produced and is related to some emulsion
properties such as droplet size, droplet surface charge
and other interfacial properties, and viscosity. In gen-
eral, emulsions with weaker stability result in encapsu-
lated powders with higher surface oil contents and a
lower retention of volatiles.[62,63] Many studies have
 Table 1. Spray drying for the encapsulation of bioactive compounds.
Inlet Outlet
Encapsulating temperature temperature
ingredient Wall material (°C) (°C) Purpose Reference
β-Carotene Casein sodium salt 110 80 Improve storage stability of β-carotene [41]
Cinnamon oleoresin Gum arabic/maltodextrin/modified starch 160 120 Improve stability of volatiles during storage [42]
Curcumin WPI 150, 110 NR Improve solubility and bioavailability of curcumin [43]
D-Limonene β-CD 200 NR Evaluate release profile of D-limonene under different humidity and temperature [6]
conditions
Egg powder Gelatin, lactose, pullulan, and their mixtures 171.8 72.5 Improve oxidation stability during storage [44]
Elderberry Gum arabic, maltodextrin, isolated soya protein, soya 80 NR Enhance stability of the phenolic content and color of the powder [45]
(Sambucus nigra protein powder, soya milk powder
L.) juice
Elemi and Maltodextrin 150 80 Analysis of essential oils components [46]
peppermint oils
Flaxseed oil Maltodextrin/gum arabic or WPC or modified starch 180 110 Protection against lipid oxidation [47]
Gac oil Blend of WPC and gum arabic 150 95 Preservation of color and carotenoid, lycopene content [48]
Juçara pulp Gelatin, gum arabic, and maltodextrin 165 NR Retention of anthocyanin content [49]
Lippia sidoides Gum arabic, maltodextrin 160 NR Improve antifungal activity of essential oil [50]
essential oil
Lycopene Gelatin/sucrose 190 52 Storage stability to avoid the damage from oxygen and light during storage [21]
Lycopene Maltodextrin 147 NR Enhance storage stability of lycopene [22]
Mandarin oil Gum arabic/maltodextrin 200 80 Retention of volatiles [51]
Peppermint oil Maltodextrin 150 80 Characterization of water vapor sorption properties [14]
Pequi pulp extract Gum arabic 152 NR Retention of high vitamin C and carotenoid content [31]
Persimmon pulp Maltodextrin, gum arabic, starch sodium octenyl 110 85 Efficient powder recovery and retention of phenolic content [52]
succinate, WPC, and egg albumin
Pomegranate juice Maltodextrin 100 NR Reduction of the stickiness of the products, retention of anthocyanin and phenolic [53]
content
Tamarind pulp Maltodextrin/soya protein isolate 170 NR Reduction of maltodextrin required for the production of tamarind pulp powder using [54]
soya protein isolate, enhancement of quality of tamarind pulp
Tomato oleoresin Soy protein isolate/gum arabic 140 55–60 Control release, increase stability of lycopene and maintenance of color [55]
NR, not reported; WPI, whey protein isolate; β-CD, β-cyclodextrin; WPC, whey protein concentrate.

143
144 C. G. DROSOU ET AL.
demonstrated that the reduction in size of the emulsion
droplets results in greater retention of volatiles and
lower surface oil.[64–66] According to Jafari et al.,[19]
the higher surface oil in the particles produced from
emulsions with larger droplets can be attributed to
droplet breakdown during atomization. The reduction
in size can be achieved, for example, using high-press-
ure homogenization or by increasing the emulsion vis-
cosity or decreasing the oil load. For instance, in a
microencapsulation process of flaxseed oil by spray dry-
ing, lower oil content resulted in higher emulsion
viscosity.[67] Many authors reported that an increase
in emulsion viscosity generally reduces the time needed
to form a semipermeable membrane or an outside shell
in the atomized droplets at the early stages of the drying
process.[19,39,60] According to Huynh et al.[39] and
Tonon et al.,[67] the membrane formed around the
droplet surface becomes impermeable to larger com-
pounds such as flavors and oils, thus reducing the oil
migration to the particle surface.
Encapsulation of bioactive compounds by
spray drying
Spray drying is the most commonly used encapsulation
technology in the food industry and is considered as a
cost-effective way to produce microcapsules in a rela-
tively simple and continuous processing operation.[68]
Since the main purposes of microencapsulation are to
protect sensitive components in solid carriers, to reduce
volatility, to promote easier handling, and to control the
release of the encapsulated material during storage and
in applications,[69] the selection of an appropriate wall
material is critical to the encapsulation efficiency by
spray drying.[70] Depending on the core material and
the characteristics desired in the final product, wall
materials can be selected from a wide variety of natural
and synthetic polymers. Among the available ingredi-
ents, the major wall materials used for spray drying
applications are carbohydrates, including modified
and hydrolyzed starches, cellulose derivatives, gums
(exudates, extracts, etc.), and cyclodextrins as well as
proteins including whey proteins, caseinates, and
gelatin.[19] The wall material must be soluble in water
as almost all spray drying processes in the food industry
are conducted using an aqueous feed formulation as
well as should have film forming and good emulsifi-
cation properties, and finally the wall concentrated
solutions should be of low viscosity.[70,71] For instance,
carbohydrates, with the exception of gum arabic, lack
active surface properties and must be used in conjunc-
tion with emulsifying agents to encapsulate hydro-
phobic core materials;[72] among the polysaccharides
used, gum arabic solutions are of relatively low viscosity
even at high polymer concentrations On the other hand,
proteins are surface active and have the ability to form
films at the interface and stabilize emulsion droplets;
as a result, in many studies, blends of carbohydrate
and proteins are being used.[8] In addition, the incor-
poration of hydrolyzed carbohydrates (maltodextrins,
oligosaccharides) into the wall system has been shown
to improve the drying properties of the wall matrix,
probably by enhancing the formation of a dry crust
around the drying droplets and increasing the oxidative
stability due to reduced oxygen permeability.[73]
In recent decades, lipophilic bioactive components,
such as oils and carotenoids, have been gaining great
public interest globally due to their health benefits.
However, oils, containing a high amount of omega-3
fatty acids, are highly susceptible to oxidation; oxidation
of omega-3 fatty acids leads to peroxide formation and
finally to volatile compounds, some of which produce
off-flavors and ultimately decrease the nutritional value
of omega-3 fatty acids.[74] Therefore, the encapsulation
of lipophilic bioactive components in an edible form
and their incorporation into food systems or in food
supplements has been extensively investigated by the
food industries.[75] For instance, flaxseed oil, one of
the richest sources of plant-derived omega-3 fatty acids,
has been stabilized using microencapsulation by spray
drying and the results showed that whey proteins and
sodium caseinate improved the oxidative stability of
flaxseed oil during storage.[76] In another study, the
encapsulation of flaxseed oil using a mixture of
maltodextrin with gum arabic or whey protein concen-
trate (WPC) or two types of modified starch (Hi-Cap
100TM and Capsul TA) at a 25:75 ratio was investi-
gated; with respect to encapsulation efficiency, the blend
of maltodextrin:Hi-Cap showed the best performance,
while the mixture of maltodextrin:WPC enhanced the
protection of the active material against oxidation upon
storage.[47] In addition, flaxseed oil containing crawfish
astaxanthin powder was successfully encapsulated by
spray drying using a wall system consisting of sodium
caseinate and lactose. The microencapsulation efficiency
for crawfish astaxanthin was 86.06%, which indicated
that more oil was encapsulated than displaced on the
particles’ surfaces.[77] Furthermore, Botrel et al. investi-
gated the encaspulation efficiency of fish oil using
different blends of whey protein. The use of maltodex-
trin or inulin together with whey protein is a good
alternative in the spray drying process of fish oil as
the surface oil content was 5.6, 6.5, and 7.7% for the
particles produced using whey protein:inulin, whey
protein:maltodextrin, and whey protein alone,
respectively.[70] Moreover, spray drying has been

successfully applied for carotenoid stability in oils such
as gac oil which is rich in β-carotene and lycopene.
Specifically, gac oil was encapsulated using a mixture
of WPC and gum arabic at a ratio 7/3 (w/w), as opti-
mized in a previous study,[48] and the encapsulation
efficiency of the oil, β-carotene, lycopene was 87.22,
82.76, and 84.29%, respectively under optimal con-
ditions of inlet, 154°C, and outlet temperatures,
80°C.[78] In another study, maltodextrin was used to
produce gac powder by spray drying and the results
showed that total carotenoid content and antioxidant
activity were preserved at inlet temperature of 120°C
and maltodextrin concentration of 10%.[79] Addition-
ally, encapsulation by spray drying is applied to oleore-
sins which are susceptible to degradation in the
presence of air, light, moisture, and high temperatures
and have short storage life if not stored properly.[42]
For instance, microencapsulation of cinnamon oleoresin
by spray drying helps to stabilize oleoresin by prevent-
ing against volatile losses. Gum arabic is considered to
be a better wall material for encapsulation of cinnamon
oleoresin as compared to maltodextrin, and modified
starch, although the blend of gum arabic:maltodextrin:
modified starch (4:1:1) proved to be more efficient.[42]
The microencapsulation of garlic oleoresin by spray
drying was investigated and the optimum conditions
were found to be 10% garlic oleoresin, 60% maltodex-
trin concentration, and 200°C inlet air temperature,
with maximum encapsulation efficiency of 81.9%.[80]
Furthermore, zein was used as coating material to
encapsulate tomato oleoresin by spray drying and the
results showed that zein particles could protect most
of the lycopene from being released in the stomach.[81]
Similarly, essential oils are quite susceptible to oxidation
and volatilization and therefore are encapsulated to
increase their shelf life and enable their controlled
release and the conversion of liquid flavorants into
solids.[56] The microencapsulation of the essential oil
from the fruits of Pterodon emarginatus by spray drying
using gum arabic and maltodextrin was studied. A
blend of 1:3:3.6 of oil:gum arabic:maltodextrin offered
the best protection, with 98.63% of the essential oil
being retained.[82] Spray drying microencapsulation of
Lippia sidoides essential oil was investigated using
maltodextrin and gum arabic at different ratios. The
best encapsulation efficiency was achieved at maltodex-
trin:gum arabic ratio 0:1 and a carrier:essential oil ratio
of 4:1.[50]
Recently, there is an increased demand for food col-
orants from natural sources to substitute synthetic dyes.
For example, anthocyanins are considered as potential
replacements for synthetic colors because of their
bright, attractive hue, and water solubility, which
DRYING TECHNOLOGY 145
facilitates their incorporation into aqueous food systems
as well as of possibly exerting health benefits (antioxi-
dant and anti-inflammatory effects). However, the food
industry requires effective technologies which protect
the natural pigments, due to their instability under dif-
ferent environmental stresses (light, air, humidity, and
high temperatures) and interactions with other food
constituents.[3] Currently, to accomplish this protection,
microencapsulation by spray drying is used by applying
different biopolymers as wall materials. For instance,
microencapsulation of anthocyanin pigments present
in Garcinia indica Choisy was performed with malto-
dextrins of various dextrose equivalents (DE 06, 19,
21, and 33) and other additives such as gum arabic
and tricalcium phosphate to enhance the stability of
the pigment. The microencapsulated pigment using dis-
persions containing 5.0% maltodextrin DE 21, 0.25%
gum arabic, and 0.25% tricalcium phosphate was found
to have the highest antioxidant activity (69.90%) and
anthocyanin content (485 mg/100 g).[83] In another
study, the stability of anthocyanins and antioxidant
activity of blackberry powder, obtained by spray drying,
using maltodextrin, gum arabic, or a blend of both car-
riers was studied. Maltodextrin provided greater stab-
ility for spray-dried blackberry powder, because the
particles produced with this wall material exhibited
the longest half-life and the lowest anthocyanin degra-
dation rate at 25°C.[84]
Phenolic compounds have been also attracting con-
siderable interest because of their positive effects on
human health. However, polyphenols show low water
solubility and low stability to different environmental
conditions (exposure to light, oxygen, temperature,
and enzymatic activities). For these reasons, several
microencapsulation systems have been examined to
preserve the biochemical functionalities of these
components.[85,86] For instance, Paini et al.[87] investi-
gated the encapsulation efficiency of olive pomace poly-
phenols and the highest total phenolic content was
obtained at inlet air temperature 130°C, maltodextrin
concentration 100 g/mL, and feed flow rate 10 mL/
min. In addition, peanut sprout extract, rich in resvera-
trol, was successfully encapsulated using WPC or malto-
dextrin emulsions and the stability of capsules was
investigated. The powdered peanut sprout extract
microcapsules coated with WPC exhibited high stability
during storage, over 80% at 4 and 20°C during 10-day
storage.[88] In another study, cinnamon polyphenols
were encapsulated using maltodextrin as a wall material
and the highest total phenolic content and antioxidant
activity were observed at inlet temperatures of 160
and 180°C and flow rate of 10 mL/min.[89] Finally,
retention of elderberry juice polyphenols was enhanced
146 C. G. DROSOU ET AL.

by encapsulation through spray drying using as coating attractive forces originating from the surface tension.
materials soya milk powder, soya protein powder, iso- Beyond a critical voltage, the repulsive forces overcome
lated soya protein, gum arabic, and maltodextrin. the surface tension of the solution and an electrically
Among these wall materials, gum arabic and maltodex- charged liquid jet erupts from the tip of the spinneret.
trin gave better results at the inlet temperature of 80°C As the charged jet accelerates toward regions of lower
and a feed flow rate of 180 mL/h.[45] potential, the solvent evaporates, while the molecular
entanglements (interchain associations) among the
polymer chains prevent the jet from breaking up. This
Principles of electrohydrodynamic techniques results in ultrathin fiber formation. Generally, a
grounded or an oppositely charged plate is used to guide
The electrohydrodynamic processes use electrostatic
to the collector the spinning jet.[92–94] The difference
forces to produce electrically charged jets from viscoe-
between electrospinning and electrospraying which
lastic polymer solutions which on drying, by the evapor-
may be considered as “sister” technologies is based on
ation of the solvent, produce ultrathin structures.[90] In
concentration and viscosity of the polymer solution.[9,95]
particular, the technique is referred to as electrospin-
Generally, the viscosity increases with the concentration
ning when ultrathin continuous fibers are generated,
and chain stiffness of the polymer in solution. If the vis-
whereas when size-reduced capsules are produced, the
cosity is high enough, a stable elongated jet can be
technique is called electrospraying. The typical setup
obtained. An increase in the viscosity of the solution
for electrospinning and electrospraying consists of four
promotes a high cohesion and entanglements between
main components: (i) a high-voltage source (1–30 kV)
the polymeric chains which prevent the liquid from
usually operated in direct current mode, though alter-
breaking up into droplets, and thus a transition from
nating current mode is also possible, (ii) a blunt-ended
electrospray to electrospinning occurs. In other words,
stainless steel needle or capillary, (iii) a syringe pump,
particles will be formed if the polymer solution has a
and (iv) a grounded collector, either in the form of a flat
low viscosity or low polymer concentration, but fibers
plate or a rotating drum (Fig. 2a and 2b). The apparatus
will be formed if a higher viscosity or a higher concen-
of the process could be vertical or horizontal.[91] Both
tration solution is being used.[96] Recently, electrohy-
techniques work on the same principle with very minor
drodynamic processes are used for the encapsulation
differences. Concerning the electrospinning process, it
of bioactive compounds for food applications. Similarly
involves the application of a strong electrostatic field
with the spray drying process, encapsulation is achieved
by high voltage across a conductive capillary, attached
by dissolving, emulsifying, or dispersing the core sub-
to a reservoir containing a polymer liquid, and a screen
stance in an aqueous solution of the wall material,
collector. Upon increasing the electrostatic field
followed by spraying or spinning of the entire solution.
strength up to a critical value, charges on the surface
The novelty of the electrohydrodynamic processes is
of a pendant drop destabilize the shape of the solution
that they can be performed in two different ways, either
stream at the exit side from partially spherical into coni-
through a coaxial electrohydrodynamic process or
cal, i.e., the so-called Taylor cone effect. Two electro-
through direct incorporation of the material within
static forces play an antagonist role in this context:
the polymeric solution (cosolubilization of core and wall
The electrostatic repulsion between the surface charges
materials in the solvent) depending on the nature of the
generated by the applied voltage that tends to break
materials used (molecular compatibility). Specifically, in
the polymer solution drop at the spinneret and the

Figure 2. Schematic of setup of electrospinning (A) and electrospraying (B) apparatus.


the coaxial methodology, the polymer and the core
material are introduced into the electrohydrodynamic
equipment from separated solutions; thus, the compo-
nent immiscibility problem is alleviated.[97]
Parameters influencing fiber characteristics in
the electrospinning process
The electrohydrodynamic process has been attracting
considerable attention for the production of polymer
fibers or particles as it can generate them with diameters
in the range from several micrometers down to tens of
nanometers.[98] It is well known that fiber or particle
diameter and morphology are strongly dependent on a
number of parameters.[90] These include intrinsic
properties of the polymer solution such as type of poly-
mer, conformation of the polymer chain, viscosity, elas-
ticity, electrical conductivity, polarity, and surface
tension of the liquid dispersion. Moreover, operational
conditions such as the strength of the applied electric
field, the distance between spinneret–collector and the
feeding rate of the polymer solution are known to influ-
ence the fiber or particle characteristics. Other variables,
such as the humidity and temperature of the surround-
ings may also play an important role in determining the
morphology and the diameter of the electrospun struc-
tures as well as their physical state.[92,99–103] The proces-
sing parameters of electrohydrodynamic process are
given in Table 2.
Polymer concentration and solution viscosity
Initially, the solution viscosity is a critical factor that
influences solution spinnability and morphology of the
electrospun fibers. Viscosity is directly related to con-
centration, molecular weight, and the structure and
conformation of the polymeric chains as well as solvent
type.[104,105] Generally, an increase in viscosity increases
fiber diameter and uniformity.[100,106] The effects of zein
solution’s concentration and viscosity on electrospun
fiber morphology and size were investigated and the
authors report that beadless and uniform fibers were
Table 2. Processing parameters in electrohydrodynamic
processes.
Solution properties Viscosity
Polymer concentration
Molecular weight of polymer
Surface tension
Electrical conductivity
Processing conditions Applied voltage
Flow rate
Tip to collector distance
Ambient conditions Temperature
Humidity
DRYING TECHNOLOGY 147
noticed at higher concentrations of zein, while the
average diameter of the electrospun fibers
increased.[92,104,107,108] In addition, b-cyclodextrin
(b-CD)/poly(vinyl alcohol) (PVA) blend fibers were
produced by the electrospinning process and the effect
of b-CD concentration on fiber morphology was exam-
ined. The viscosity of b-CD/PVA solution increased
with the concentration of b-CD and it was noted that
the high viscosity of b-CD/PVA solution led to forma-
tion of more uniform nanofibers with larger average
diameter. The same trend was observed for PVA/
chitosan blend nanofibers.[109] As far as molecular
weight of the solubilized polymeric chains, Deitzel
et al.[100] and Geng et al.[110] showed that very low-
molecular weight polymers have a tendency to form
beads rather than fibers, whereas high-molecular weight
polymers give fibers with larger average diameter if the
concentration of the polymer is adequate, presumably
due to more extensive interchain associations.
Surface tension
The surface tension of a liquid dispersion, being a func-
tion of composition (solvent and dissolved constituents)
and temperature, plays a critical role in the electrospin-
ning process.[99] It is the primary counteracting force to
the charge effects generated by the applied voltage dur-
ing the electrospinning process and determines the
overall electrospinnability of the liquid medium.[111]
Surfactants are often used for electrospinning fibers to
improve the electrospinnability, to reduce the electro-
spun fiber diameter, to eliminate the formation of
beaded fibers, and to form core–shell fibers by emulsion
electrospinning.[112] The influences of surfactants on the
diameter size and uniformity of electrospun poly(L-lac-
tic acid) fibers were examined by adding various surfac-
tants (cationic, anionic, and nonionic), and significant
diameter reduction and uniformity improvement were
achieved in this way.[113] In addition, blend solutions
of chitosan and poly(ethylene oxide) (PEO) at different
acidities and in the presence of surfactant Tween 20
were electrospun to produce membranes of nanofibers
with different diameters. It was noted that solutions at
the highest acidity yield less beads and beaded fibers
than the others. This was attributed to an increase in
acetic acid concentration that gave viscous solutions
with lower surface tension and an adequate polymer
chain entanglement.[114] On the other hand, the effect
of Tween 20 was neither a significant factor on fiber
diameter, while Wang et al.[112] have reported that the
average diameter of the fibers decreased as the con-
centration of the nonionic surfactant, TritonX-100,
increased.
148 C. G. DROSOU ET AL.
Conductivity
The electrical conductivity of solution also plays an
important role on fiber morphology and size;[115] this
property is related to the charge density on a jet (liquid
stream), thereby affecting the extent of elongation of
the jet by the applied electrical force. Under the same
operating voltage and spinning distance, a solution with
a higher electrical conductivity may cause higher elon-
gation of a jet along its axis and thus yield electrospin-
ning fibers of smaller diameter.[116] For instance, Tan
et al.[116] investigated the effect of solvent electrical
conductivity on morphology of electrospun poly
(L-lactide-co-caprolactone) fibers using dichloro-
methane (DCM), N,N-dimethylformamide, and pyri-
dine as solvents. The results showed that electrospun
polymer nanofibers with the smallest fiber diameter
and highest uniformity were obtained from the DCM/
pyridine (50/50 wt%) solution, having the highest
electrical conductivity. The same trend was also noted
for poly(acrylic acid)[117] and polystyrene[118] fibers.
Applied voltage
The applied voltage is the critical element of any electro-
spinning process because it provides surface charge on
the electrospinning jet, and thereby influences the nano-
fiber diameter. Generally, increasing applied voltages
lead to decreasing diameters of nanofibers due to
increasing electrostatic repulsive forces on the fluid jet,-
[99,119]
e.g., for chitosan nanofibers produced by electro-
spinning it was noted that by increasing the voltage, the
diameter of nanofibers decreased.[120] However, very
high voltages may facilitate nanofibers of larger dia-
meters as increasing the voltage above a certain level
increases the electrostatic stresses, which in turn, may
draw more material out of the syringe.[103,121] For
instance, zein solutions were electrospun at different
applied voltages and the results showed that the low vol-
tages gave small fiber diameters. Specifically, an applied
voltage of 13 kV gave fiber diameters ranging from 250
to 300 nm, while a voltage 18 kV resulted in fiber dia-
meters ranging from 250 to 350 nm at different solution
feed rates.[122] In addition, bead formations can occur at
high voltages.[100,121]
Flow rate
The flow rate of the polymer from the syringe is another
important process parameter as it influences the jet
velocity and the material transfer rate. A minimum
value of solution volume suspended at the end of the
needle should be maintained to form a stable Taylor
cone and facilitate solvent evaporation.[99,123] The feed
rate therefore determines the amount of solution avail-
able for the electrospinning process. Typically, when the
feed rate increases, a corresponding increase in the fiber
diameter is observed.[124] Few studies have systemati-
cally investigated the relationship between solution flow
rate on fiber morphology and size. For instance, Okutan
et al.[111] investigated the influence of feed rate during
electrospinning on properties of electrospun gelatin
and reported that with the increasing feed rate, there
were larger fiber diameters and bead formations. More-
over, zein fibers were produced at 1.0 and 2.0 mL/h sol-
ution feed rate and the fiber diameters ranged from 250
to 275 nm and from 250 to 350 nm, respectively.[122]
Similarly, Henriques et al.[125] observed that the average
diameter of electrospun PEO fibers increases linearly
with solution feed rate.
Tip to collector distance
Another influential parameter is the distance between the
needle tip and the collector device, and this is correlated
with the flight time of the electrospinning jet. Longer
flight time may produce a thinner fiber as the fiber gets
more time to stretch and elongate before it is accumu-
lated on the collector.[126] Consequently, the fiber diam-
eter generally decreases with larger distance between
needle tip and collector.[127] Nevertheless, Lee et al.[128]
have proposed that the fiber diameter increases at a
longer distance due to reduction of the effective voltage.
Similarly, Sencadas et al.[120] instigated the influence of
the distance between the needle tip to the grounded
collector on the fiber average diameter of a 7% (w/v) chit-
osan in 70/30 trifluoracetic acid (TFA)/DCM solution. It
was observed that the fibers with the smallest average
diameter, ∼260 nm, were obtained for samples with
5 cm in distance between the needle tip and the collector
and that the mean fiber diameter increased by increasing
the distance between the needle tip and the collector. A
maximum average fiber diameter of ∼500 nm was
obtained for a traveling distance of 20 cm.[120]
Humidity and temperature
The humidity and temperature of the process can also
affect the morphology and diameter of the electrospun
fibers, although no systematic study was conducted on
the influence of evaporation and solidification of the
jet. Most investigations have been performed in an open
atmosphere without controlling the vapor concentration
of the solvent. Tripatanasuwan et al.[129] investigated the
effect of different relative humidity (5.1–63.5%) envir-
onments on PEO electrospun fiber morphology and

size. The average diameter of PEO nanofibers gradually
decreased as the relative humidity increased. The evap-
oration rate from the fluid jet decreased at higher rela-
tive humidity, which allowed the charged jet to continue
to elongate. On the other hand, more beads appeared at
higher humidities.
Parameters influencing particle
characteristics in the electrospraying process
The size and morphology of the particles prepared by
electrospraying influence the release kinetics of the
entrapped bioactive compounds. Spherically shaped
particles are considered more suitable for delivery of
bioactives than irregularly shaped particles, mainly
because of polymer dissolution and thus the bioactive
release might be inconsistent from within the irregularly
shaped particles.[130] Therefore, all the parameters that
have an impact on particle morphology and size are
discussed below.
Polymer concentration, molecular weight, and
viscosity
Polymer type, molecular weight, and concentration are
very influential factors in the electrospraying process;
i.e., changing polymer concentration and molecular
weight largely affect the viscosity and surface tension
of the solution.[131] With greater length of polymer
chains, intermolecular associations are favored, parti-
cularly as the solution concentration is raised, leading
to larger size microcapsules. For low-molecular weight
polymers, a higher concentration is required for the for-
mation of particles. In contrast, high-molecular weight
materials display a great number of entanglements,
allowing particle formation even with polymer solutions
of low concentration.[1] To have a stable process, it is
important to take into consideration the viscosity of
the polymer solution; with an increasing concentration,
the increased viscosity leads to the production of cap-
sules with bigger size. For instance, Gomez-Estaca et al.[1]
investigated the effect of zein concentration on the mor-
phology of the resulting zein structures for polymer con-
centrations ranging from 1 to 20% (w/w) in aqueous
ethanol solutions. It was found that 1% of zein in the sol-
ution was too low for particle formation, while a zein
concentration of 20% gave rise to the transition from
particles to fibers, a finding which was in accordance
with observations made in earlier work.[132] With zein
concentrations of 2.5 and 5% (w/w), the generated par-
ticles were round in shape and had relatively smooth
surfaces, whereas much larger particles in size were
obtained by increasing the polymer concentration. An
DRYING TECHNOLOGY 149
increase in particle size with higher polymer concen-
tration and viscosity has been also noted for other poly-
mers, such as polycaprolactone (PCL),[133] alginate,[134]
chitosan,[135] and elastin.[136]
Surface tension
Surface tension plays a role in the electrospraying pro-
cess, since it affects the ease of initial drop formation
as the solution gets out of the nozzle. It is worth men-
tioning that the initial drops are formed when the elec-
trostatic forces overcome the surface tension of the
emerging liquid jet, and then these initial drops explode
to smaller drops as they travel in the electrostatic field
between the nozzle (usually positively charged) and
the collector (usually negatively charged). A lower sur-
face tension leads to smaller initial drops and hence
smaller final nanoparticles. The effect of higher surface
tension on increased particle size has been reported for
solutions of amylose and amylopectin[137,138] as well as
PCL.[139]
Conductivity
The electrical conductivity of the polymer and solvent is
an important parameter when optimizing the electro-
spraying process as it affects the electrostatic attraction
of the charged particles to a grounded or oppositely
charged collector. With higher electrical conductivity,
the Coulombian repulsion forces are enhanced and
compete with the viscoelastic forces of the solution; as
a result, disentanglements in the polymer chain network
occur during electrospraying, producing smaller parti-
cles. Gañán-Calvo et al.[140] showed that a decrease in
particle size can be obtained with an increasing solution
conductivity. Nevertheless, if only conductivity had
been the parameter controlling the particle size, higher
conductivity values would have produced larger particle
dispersity due to Coulomb fission forces, which over-
come chain entanglement forces, and thereby produce
secondary droplets that are ejected from primary dro-
plets, resulting in broader particle size distribution.[141]
Correlating with viscosity, stable electrospraying can be
achieved only when viscosity is high or conductivity is
low as reported for chitosan particles.[142] Changes in
electrical conductivity can be obtained by changing
the electrospraying solvent or using cosolvents,
although this latter case may be detrimental to size dis-
tribution and morphology of the particles. For instance,
electrospraying was used to prepare poly(lactic-co-
glycolic acid) (PLGA) microparticles using two different
solvents, DCM and trifluoroethanol. Trifluoroethanol
enabled the preparation of even smaller sizes of PLGA
150 C. G. DROSOU ET AL.
particles, which can be attributed to the high conduc-
tivity of trifluoroethanol (TFE) (1.07 μS/cm) compared
to DCM (0 μS/cm).[143] In addition, PLGA particles
were produced using a mixture of DCM with chloro-
form to increase the conductivity of the solution. The
results showed that the addition of a solvent with high
conductivity destroys electrospraying stability and pro-
duces smaller and polydisperse particles. In another
study, the effect of conductivity on particle formation
was studied by adding the organic salt didodecyldi-
methylammonium bromide (DDAB) in the polymer
solution. The conductivity of a 5% (w/v) PLGA solution
in acetonitrile containing 10% (w/w) paclitaxel was
shown to increase from 0.51 to 116.5 μS/cm by the
addition of 2 mM DDAB. This led to a particle size
decrease from around 1.2 µm to 355 nm.[133]
Applied voltage
The applied voltage is a key parameter in achieving a
stable cone-jet mode for obtaining monodispersed
nanoparticles.[1] Within the single cone-jet mode, size
is not significantly affected by voltage, and only a
slight decrease in size is observed when voltage is
increased.[134,144–146] Morphology, however, will be
changed as stated by Shenoy et al.,[147] since as the volt-
age is increased, the particle morphology is largely
modified from a spherical shape to elongated particles
or beaded fibers to eventually only fibers if the polymer
concentration is sufficiently high. This is due to more
charge acting on droplets with increased voltage, lead-
ing to stretching and elongation of droplets. It is there-
fore recommended to use moderate voltages that allow
for the single cone-jet mode to take place while main-
taining the spherical morphology of the particles.[130]
Flow rate
The flow rate of the liquid stream in the electrospraying
process influences the size of the particles. Higher flow
rates could lead to a larger diameter of capsules as the
jet speed increases and higher concentration of polymer
solution drips out of the nozzle. Gomez-Estaca et al.[1]
noticed that the size of the particles decreased with
the zein solution flow rate and the nanoparticle dia-
meters were observed to lie between 80 and 130 nm
and 130 and 175 nm for the 0.05 and 0.10 mL/h flow
rate, respectively. The effect of the flow rate on the
diameter of several polymeric nanoparticles generated
by electrospraying has been reported by several authors
using polymers such as PLGA,[144,146] chitosan,[135]
elastin,[136] and PCL.[133,139]
Tip to collector distance
Electrospraying distance can also affect capsules’ size
and have an impact on the final product morphology.
In the electrospray process, once the compound jet is
formed, droplets are largely discharged by a needle con-
nected to positive voltage. The position of the spray
nozzle does affect particle size and particle size distri-
bution. The investigation of this parameter revealed that
increasing the tip–collector distance decreases the aver-
age size of particles as mentioned for amylose and
amylopectin[148] as well as for PCL.[139] This is due to
the fact that a longer flight of droplets in the electric
field, as a result of longer tip–collector distance, pro-
vides more time for further coulomb explosions, and
as a result smaller particles are being formed. In
addition, increasing the distance leads to more spherical
morphologies since polymer chains have sufficient time
to diffuse within the droplet and thus also reduced
polydispersity.[130] It must be pointed out, however, that
increasing the tip–collector distance to more than a
threshold will lead to disruption of drop breakage
because of too weak electrical field.[148]
Blends of polymers used in
electrohydrodynamic process
There has been growing interest in the development of
natural polymer-based nanofibers. Compared to nanofi-
bers prepared from synthetic polymer solutions by elec-
trospinning, bionanofibers have remarkable advantages
in terms of high crystallinity, uniformity, biodegradabil-
ity, and biocompatibility.[149] However, electrospinning
of nanofibers from biopolymers has proven to be quite
challenging because these materials have limited solu-
bility in most organic solvents, are often polyelectrolytes
when dissolved, have poor molecular flexibilities, readily
form three-dimensional networks through hydrogen
bonding, and most importantly are insufficiently
entangled to facilitate electrospinning.[150] Therefore,
researchers have focused on the use of composite blends
of biopolymers with polymers that are compatible for
formation of electrospun fibers with enhanced material
properties such as higher tensile strength.[151] Synthetic
polymers such as PEO and PVA, when combined with
biopolymers, improve the fiber forming ability of the
blending solution.[152] For instance, chitosan-based
nanofibers have been successfully electrospun from
chitosan solutions blended with PEO,[153] PVA,[109,149]
and silk fibroin.[154] Similarly, sodium alginate fibers
have been fabricated by electrospinning of aqueous mix-
tures in the presence of PVA[155–157] and PEO.[158,159] In
addition, collagen was blended with PEO to produce

electrospun fibers.[160] In addition to synthetic poly-
mers, there has been a lot of interest in the study of
polymer blends, especially focused on biodegradable
and sustainable materials. Increasing attention has been
given in recent years to natural polymers, such as poly-
saccharides, due to their abundance in nature, unique
structures, and characteristics with respect to synthetic
polymers.[161] This renaissance of polysaccharide mate-
rials is influenced by their useful properties including
nontoxicity, biocompatibility, biodegradability, and
water solubility, making these biopolymers suitable for
different applications. Several polysaccharides, includ-
ing starch, pectin, cellulose, chitin, and chitosan, have
been finding new potential uses in the food field. Chit-
osan is the second most abundant biological polysac-
charide (after cellulose) derived from nature and this
material finds many applications due to its unique
properties, such as antibacterial performance under cer-
tain specific conditions.[162] Nevertheless, fiber forma-
tion from chitosan by electrospinning on its own is
rather difficult because of its limited solubility and poly-
cationic nature in solution. Therefore, Torres-Giner
et al.[163] used blends of zein with chitosan to develop
novel antimicrobial materials which have potential for
applications in different fields such as active and bioac-
tive packaging, antimicrobial food coatings, etc.
Furthermore, zein nanofibers containing cyclodextrins
(α-CD, b-CD, c-CD) were produced through electro-
spinning and the results showed that the addition of
cyclodextrin in the polymer solutions improves the elec-
trospinnability of the zein nanofibers at lower polymer
concentration. Thermal analyses showed that zein/
b-CD nanofibers have higher glass transition tem-
peratures and higher degradation temperature with an
increasing cyclodextrin content. In another study, novel
ultrathin electrospun fibers from different blends of
amaranth protein isolate and the microbial polysacchar-
ide pullulan were developed. The presence of pullulan
(neutral polysaccharide with flexible conformation in
aqueous solutions) in the blends resulted in increased
viscosity and lower conductivity of the solutions; these
led to improved chain entanglements and weakening
of the polyelectrolyte character of the protein compo-
nent, both favoring fiber formation.[164] Another work
described the electrospinning of zein/hyaluronic acid
blend fibrous membranes, where, to enhance compati-
bility between the protein and the polysaccharide
components, poly(vinyl pyrrolidone) was introduced
into the aqueous ethanol solutions of the blend.[165]
The use of food hydrocolloids complicates the elec-
trospraying process, since these materials may consist
of low-molecular weight polymers which do not gener-
ate sufficient viscosity and they generally exhibit strong
DRYING TECHNOLOGY 151
intermolecular and intramolecular forces, which need to
be somehow counteracted to promote capsule forma-
tion. In addition, the use of aqueous solutions further
complicates the process due to the ionization of water
molecules at high voltages in an air environment, which
may cause corona discharge. Moreover, aqueous solu-
tions present high-surface tension values which hinder
the formation of stable liquid fluid jets during the
process.[166,167] One way to reduce the high surface ten-
sion of aqueous solutions to stabilize the electrospraying
process is the use of surfactants. Surfactants are used in
a wide array of applications because of their potential to
lower surface or interfacial tension of the medium in
which they are dissolved.[168] For instance, capsules of
low-molecular weight carbohydrates (e.g., maltodextrin,
resistant starch) were obtained by use of the surfactants
Tween 20, Span 20, and lecithin.[169] In another study,
gums and surfactants were used to modify the aqueous
hydrocolloid dispersion properties allowing capsule for-
mation through electrospraying. The results showed
that the use of nonionic surfactants was the most inter-
esting strategy for improving the sprayability of these
materials, since gums retained too much solvent that
led to aggregated and wrinkled particles.[168]
Encapsulation of bioactive compounds by
electrohydrodynamic process
The growing consumer’s interest for the promotion of
health and disease prevention through improved
nutrition has led to numerous attempts to develop
food-grade delivery systems, including active packaging,
to encapsulate, protect, and controlled release of bioac-
tive components.[170–172] More specifically, natural
compounds with antimicrobial features are of great
interest for the active packaging industry and their
efficient encapsulation and controlled release represent
a major challenge considering their sensitivity to heat,
oxygen, and light. Recently, electrospinning has been
receiving great attention in functional food and active
food packaging systems.[173,174] This relatively simple
technique can be applied for the production of nanofi-
brous polymeric membranes (coating films) formed by
polymer fibers. Electrospun nanofibers exhibit proper-
ties such as high porosity, large surface area per unit
mass, high gas permeability, and small interfibrous pore
size, with most of these properties being quite important
when these materials are used as carriers for delivery of
bioactive compounds.[175,176] In the literature, few
works are focused on electrospinning of edible
biopolymers,[132,177] and even less on edible polysac-
charides for controlled release of bioactives. In general,
polysaccharides do not need toxic solvents to be
152 C. G. DROSOU ET AL.
electrospun[167] and are commonly used in food appli-
cations as coating and thickening agents, or additives
for technological aims. Common polysaccharide-based
wall materials used in electrospinning and electrospray-
ing are pullulan, chitosan, alginates, dextrans, cellulose,
and its derivatives. For instance, a blend of edible carbo-
hydrate polymers (pullulan and cyclodextrin) was used
to encapsulate antimicrobial aroma compounds for
enhancing microbial safety of food products. The
release of aroma compound was negligible at ambient
conditions (23°C and 55% RH), even at high tempera-
tures (up to 230°C), but it occurs beyond a given relative
humidity threshold (90%),[178] presumably due to water
plasticization of the carbohydrate matrix and the
underlying enhancement in molecular mobility of the
encapsulated components. In addition, folic acid has
been encapsulated through electrospinning in amaranth
protein isolate:pullulan ultrathin fibers with very high
encapsulation efficiency (>95%). Encapsulation within
the amaranth protein isolate:pullulan structures
increased the thermal stability of folic acid and no degra-
dation of it was observed after 2 h of UV exposure.[179]
Similarly, amaranth protein isolate:pullulan ultrathin
fibers were used to improve the antioxidant characteris-
tics of two bioactive phenolic compounds, quercetin and
ferulic acid, during an in vitro digestion protocol.[10] The
authors reported that the encapsulated bioactive com-
pounds kept their antioxidant capacity to a greater
extent in comparison with the nonencapsulated ones
during in vitro digestion.[180] Moreover, other research-
ers have focused on the use of proteins as wall materials
for the encapsulation of active compounds. Common
proteins used as encapsulating materials in electrospin-
ning are WPC, whey protein isolate (WPI), soy protein
isolate, zein, gelatin, and casein. In this context, electro-
spinning of zein (prolamine) shows an excellent outlook
for its application in the stabilization of light and
oxygen-sensitive food components;[181] zein is a hydro-
phobic protein (prolamin) extracted from corngrains,
and is known for its high thermal resistance and great
oxygen barrier properties. Fernandez et al. (2009)
encapsulated β-carotene, a good source of provitamin
A with antioxidant properties, in ultrafine zein fibers
through electrospinning and showed that the encapsu-
lated β-carotene was stable and well dispersed within
the zein fiber matrix. The electrospun β-carotene had
significantly higher light stability than the nonencapsu-
lated control.[182] In addition, gallic acid had retained
its antioxidant activity after incorporation in zein
electrospun fibers.[183] Li et al.[132] encapsulated ( )-
epigallocatechin gallate in electrospun zein fiber to
stabilize the polyphenol during simulated food proces-
sing conditions. The authors report that successful
immobilization of ( )-epigallocatechin gallate occurred
when the fibers were aged for at least 24 h under dry
conditions at ambient temperature. Moomand and
Lim[184] encapsulated fish oil, rich in omega-3 fatty
acids, in zein fibers and the results indicated that electro-
spun zein fibers provide a greater oxidative stability in
comparison to nonencapsulated fish oil. These studies
showed that electrostatic encapsulation processes are
very versatile for preparing a zein-encapsulant polymeric
matrix to protect bioactive compounds. Furthermore,
electrospun soy proteins have been used for controlled
release of allyl isothiocyanate.[185]
On the other hand, electrospraying has been widely
used to generate micro, submicro, and nanocapsules
for several applications in the area of encapsulation of
bioactive compounds.[186] Biopolymer-based particles
are used to protect and deliver bioactive compounds
in food systems or as fat replacers in foods by simulat-
ing the rheological, optical, and sensorial properties of
lipid droplets. For food applications, capsules are gener-
ally preferred rather than fibers, since apart from facil-
itating better handling and subsequent incorporation
into different products with minimal effects on sensorial
attributes, they usually present greater surface/volume
ratio and, thus are expected to have better release pro-
files than fibers.[146] Therefore, there has been consider-
able interest in the formation of biopolymer particles
from proteins and/or polysaccharides.[187] Recent
works have demonstrated that it is possible to obtain
hydrocolloid-based encapsulation structures using elec-
trospraying through proper adjustment of the process
parameters and/or changing the solution properties
through the addition of proper additives.[168,169] For
instance, WPC micro, submicro, and nanocapsules were
produced through electrospraying from aqueous
solutions for the encapsulation of the antioxidant β-
carotene. The results demonstrate that changes in pH
of the solution have an impact on polymer confor-
mation and capsule size, with larger capsules being
obtained at pH 6.4. Moreover, the capsules were
effective in stabilizing the β-carotene against photo-
oxidation as very high encapsulation efficiencies were
achieved.[10] Electrospraying was also evaluated for the
encapsulation of folic acid using both a WPC matrix
and a commercial preparation of resistant starch.
Greater encapsulation efficiency was observed using
WPC as wall material and the WPC protected the folic
acid against degradation during storage, especially
under dry conditions. In another study, curcumin,
a food colorant with low solubility in water, was
encapsulated in gelatin matrix, and the water solubility
and bioaccessibility were significantly improved by
encapsulation.[188] Similarly, lycopene was encapsulated
 DRYING TECHNOLOGY 153

through electrospraying within different edible biopoly-
meric matrices (dextran, WPC, and chitosan); it was
seen that WPC presented the greatest encapsulation
efficiency (around 75%) and the WPC capsules were
also able to better protect lycopene against moisture
and thermal degradation.[189] Torres-Giner et al.[190]
encapsulated docosahexaenoic acid (DHA) in zein cap-
sules using an electrospraying process; the encapsulated
DHA showed enhanced chemical stability against
degradation under different environmental conditions
such as relative humidity and temperature and reduced
off-flavor notes. In another study, gelatin, WPC, and
soy protein isolate were compared as emulsion stabili-
zers and wall matrices for encapsulation of a-linolenic
acid. The results showed that the WPC and soy protein
isolate capsules significantly delay the degradation of a-
linolenic acid at 80°C.[191] Extensive lists of applications
of electrospinning and electrospraying as techniques for
the encapsulation of bioactive compounds are presented
in Tables 3 and 4, respectively.
Future needs
The food industry becomes more integrated with
nutritional sciences due to current consumer demand
for natural and healthy products; therefore, it guides
and facilitates new processing approaches, including
encapsulation technologies, for the enrichment of food
matrices with bioactive compounds. Generally, encap-
sulation has been used to protect bioactive compounds
in food systems from adverse environmental factors and
to facilitate the control release at the targeted site. Spray
drying is a well-established industrial process for the
continuous production of dry powders and has been
widely used for the encapsulation over the past few dec-
ades. However, in spite of the recent developments, the
process remains far from completely being controlled.
In the spray drying process, the final properties of the
particles (e.g., size, size distribution, and morphology)
as well as the efficiency of encapsulation are affected
by process parameters and solution properties; as a
consequence, an extensive set of trial and error experi-
ments are required for the production of microstruc-
tures with desirable characteristics. Therefore, future
research needs to be focused on establishing a well-
defined link between the solution properties, process
parameters, and particle microstructure performance.
Moreover, a great work remains to be made concerning
the choice of encapsulating materials according to the
chemical and physical nature of the core and wall
material, the interaction (compatibility) between those
as well as their relative proportion in the formulation
of the capsules. In addition, the screening of new wall
biopolymers, which could ensure both the effective
preservation of functional components and the modu-
lated release of the core ingredient, becomes essential
to replace overly used materials such as gum arabic
and maltodextrins.
In recent years, electrospraying and electrospinning
have attracted researchers’ interest due to their possible
applications in food materials. These electrohydrody-
namic processes have shown great potential for making
micro and nanosized particles and fibers and lately are
being used for encapsulating bioactive compounds.
Nevertheless, the potentialities of fibers and particles
have not been widely explored in food-related

Table 3. Electrospinning technique for the encapsulation of bioactive compounds.

Encapsulating ingredient Wall material Size range studied Purposes Reference
β-Carotene Zein prolamine 1,140 nm Enhance stability against UV irradiation [182]
β-Carotene-loaded PVA, PEO 407.9 ⌃ 138.6 nm (PVA), Enhance stability against UV irradiation [192]
nanoliposomes 379.7 ⌃ 118.8 nm (PEO)
Allyl isothiocyanate Soy protein isolate /PEO, 200 nm–2 µm Control release, enhance antimicrobial activity [193]
poly(lactic acid)
Cinnamaldehyde Chitosan/PEO ∼50 nm Enhance antimicrobial activity [194]
Curcumin Zein 310 nm Improved sustained release and effective free [195]
radical scavenging ability
Fish oil rich in omega-3 Zein 190–500 nm Increase oxidative stability of fish oil [184]
fatty acids
Gallic acid Zein 327–387 nm Evaluate thermal stability and retention of [183]
antioxidant activity
Magnesium L-ascorbic Polyacrylonitrile 200 ⌃ 15 nm Examine in vitro release characteristics [196]
acid 2-phosphate,
α-tocopherol acetate
Perillaldehyde Pullulan/β-CD ∼250 nm Control release of aroma compound [178]
Quercetin and ferulic acid Amaranth protein isolate: 260.8 ⌃ 73.2 nm, Evaluate release characteristics and protection [180]
Pullulan 362.6 ⌃ 94.4 nm ability of antioxidant compounds during
in vitro digestion, enhance thermal stability
R-(á)-limonene Pullulan/β-cyclodextrin 370 nm Increase storage stability, control release [197]
Vanillin PVA/cyclodextrin 120–230 nm Prolong shelf life, enhance high temperature [177]
stability
PVA, poly(vinyl alcohol); PEO, poly(ethylene oxide).
154 C. G. DROSOU ET AL.
Table 4. Electrospraying technique for the encapsulation of bioactive compounds.
Encapsulating ingredient Wall material
α-Linolenic acid Gelatin, WPC, and soy
protein isolate
β-Carotene WPC
Bovine serum albumin Poly(D,L-lactide-co-
glycolide)
Curcumin Zein
DHA Zein
Ethylvanillin Ethylcellulose
Folic acid WPC and commercial
resistant starch
Lycopene Dextran, WPC, and
chitosan
Maltol flavor Stearic acid/ethylcellulose
WPC, whey protein concentrate; DHA, docosahexaenoic acid.
applications by the industry as more research is needed
to optimize the operating conditions and solution
properties for effective encapsulation of various bioac-
tives. For incorporation of such composite structures
within food matrices, the use of food hydrocolloids as
encapsulating matrices is highly preferred, not only
for achieving a better integration of the capsules in
the foodstuffs but also for improving consumer percep-
tion for these formulations. However, the use of biopo-
lymers (e.g., natural food hydrocolloids) often
complicates the electrohydrodynamic processes, due to
their poor viscoelastic behavior in solution, lack of suf-
ficient molecular entanglements, and limited solubility;
therefore, more research is needed to modify solution
properties to enhance the spinning or spraying of food
grade biopolymers. The selection of appropriate carriers
needs to be further explored, in conjunction with the
nature of the bioactive compound, so as to overcome
compatibility, stability, and bioavailability hurdles.
Another complicating issue for the use of electrohydro-
dynamic processes is the multitude of optimizable fac-
tors. Only a few processing parameters can be
controlled directly as some of the parameters involved
are either highly interdependent or derive from the
properties of the used polymeric solutions. In addition,
a big challenge for such processes remains the scaling
for industrial purposes. Nowadays, these techniques
have been successfully used on laboratory scale but their
low throughput restricts their commercial exploitation
at a larger scale. Specifically, the throughput of a single
electrohydrodynamic setup is inherently low, owing to
the relatively low flow rates adopted in the process,
which are in the range of microliters per minute. One
way to increase the production and simultaneously to
compete with cost-effectiveness of the spray drying
processes would be the development of an array of
Size range studied Purposes Reference
Nano-, submicro, and microcapsules Increase oxidative stability under thermal [191]
were obtained treatment
<100 nm Increase stability of the WPC capsules [10]
containing β-carotene against photo-
oxidation
3.0–5.5 µm Decrease the degradation rate of the [198]
susceptible protein
175–250 nm Enhanced stability and dispersion in aqueous [199]
food matrix
500–700 nm Improve stability [190]
45–85 nm Evaluate release profile of bioactive [200]
component
Nano, submicro, and microcapsules Increase stability of folic acid under different [201]
were obtained conditions
0.8 ⌃ 0.3 µm (dextran), 2.1 ⌃ 0.7 µm Protect lycopene against moisture and [189]
(WPC), 0.2 ⌃ 0.1 µm (chitosan) thermal degradation
10–100 nm Limit flavor degradation or loss during [202]
processing and storage
nozzles. Finally, despite the differences between the
principles of both encapsulation techniques, several
common research needs can be identified, concerning
the improvement on encapsulation efficiency and
process optimization. In more detail, there is a need
to enhance our understanding on interactions of core
and wall materials as well as on the relationships
between solution properties, process parameters, and
functionality of the powder particles derived from these
two techniques. It is thus important to explore the rela-
tions between particle microstructure, dispersibility,
stability of the core material (upon storage in different
environments and under conditions encountered in
the gastrointestinal track), and controlled release
phenomena of the entrapped ingredients. As more
information concerning structure–function relation-
ships of such deliver systems becomes available, it
would be feasible to produce tailor-made microcapsules
for fortification of functional products with bioactive
components.
Conclusion
In this review, spray drying and electrohydrodynamic
encapsulation technologies in food-related applications
were discussed. The use of these technologies for the
encapsulation of food bioactive compounds aims to
improve their stability and controlled release properties.
The encapsulation efficiency, morphology, and micro-
structure of the carrier structure are mainly affected
by the process parameters and polymer solution charac-
teristics. Although, spray drying has been a common
processing tool till now with a wide range of applica-
tions in the food industry, the emerging electrohydrody-
namic processes are gaining popularity lately due to
their high encapsulation efficiency and their ability to

better preserve heat- and oxidation-sensitive ingredi-
ents. However, further advancements in the field of
electrohydrodynamic techniques are required to
broaden their application range for microencapsulation
of bioactives in the food and pharmaceutical industries.
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