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Drying Technology

An International Journal

ISSN: 0737-3937 (Print) 1532-2300 (Online) Journal homepage: http://www.tandfonline.com/loi/ldrt20

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

Accepted author version posted online: 30


Mar 2016.
Published online: 30 Mar 2016.

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Download by: [Institut Agroquimica Tecnologia] Date: 05 July 2017, At: 01:31
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- addition, spray drying ensures microbiological stability
tions which on drying, by evaporation of the solvent, of the products, reduces the storage and transport costs,
produce ultrathin polymeric structures of varying and minimizes the risk of chemical and/or biological
morphologies.[10] The most interesting advantage of degradations by decreasing water content and water
electrohydrodynamic processes is that they can achieve activity.[7] Although spray dryers are widespread in the
high encapsulation efficiencies without application of food industry, there are two limitations of this technique.
heat treatment. The absence of heat in any electrohydro- Specifically, the carrier material should be film forming
dynamic process is a key advantage over spray drying and soluble in water and the active substance should be
and is important for preserving the structure and efficacy heat resistant at the temperatures usually applied for this
of the bioactive substances upon processing storage and drying method during the relatively short exposure to the
delivery.[11] However, its potential in the field of food hot air stream.[14] Encapsulation by spray drying involves
science is less explored thus the operating conditions several steps as shown in Fig. 1. First, the active substance
for encapsulation of food bioactives as well as the proper- to be encapsulated is homogenized with the carrier
ties and efficiency of the structures obtained have to be material at a given ratio in a liquid medium, usually an
analyzed to improve and broaden the application range aqueous phase. The mixture or emulsion that constitutes
of these emerging technologies in the food industry. As the feed solution is then pumped into the drying chamber
for every encapsulation technique, there is an optimal through a nozzle. Upon exit from the nozzle tip, the dro-
combination of process parameters, including polymer plets are atomized and come into contact with the drying
solution characteristics, to obtain composite structures fluid, i.e., hot gas (often air) inside the drying chamber.
with desirable characteristics and high encapsulation Subsequently, water is evaporated by the stream of hot
efficiency. Hence, the current review aims to present air and when the droplet water content reaches a critical
the principles and the parameters that affect the particle value, a dry crust is formed on the droplet surface and the
or fiber morphology as well as the encapsulation wall material covers the microparticles of the active
efficiency obtained from both spray drying and electro- material. If the droplet shrinks very slowly, the dry crust
hydrodynamic techniques with an emphasis on food can also develop at inner regions of the droplet and poss-
ingredient applications. Moreover, it includes the state ibly leads to the formation of a full particle. In the case of
of the art of encapsulation of food bioactives by using faster water evaporation, a crust is rapidly formed on the
each encapsulation method. 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
Principles of spray drying the bottom of the dryer or in the powder collector of
Spray drying is the oldest and the most widely used the cyclone.[14–17]
encapsulation technique in the food industry sector. It
is a flexible, continuous, and economical operation that
Parameters influencing particle
produces particles in the range from a few microns to tens
characteristics and encapsulation efficiency in
of microns with narrow size distribution.[7,12] Encapsula-
the spray drying process
tion by spray drying protects, stabilizes, and enhances the
solubility and controlled release of the bioactive com- Spray drying, being the most common method of
pounds which are delivered in a powder form.[13] In encapsulating food ingredients, is used for coating or

Figure 1. Schematic of emulsion preparation (A) and spray drying apparatus (B).
DRYING TECHNOLOGY 141

entrapping a functional component within a suitable prepared at a higher temperature had higher stability
inert carrier matrix.[18] Actually, great interest is found against the release and oxidation of D-limonene than
in encapsulation of flavors, lipids, phenolic compounds, that of the powder obtained at lower temperature. The
and colorants, including carotenoids. Successful encap- findings may be partly attributed to an increase in shell
sulation of functional ingredients should result in a thickness of the particle at higher temperatures. The
powder with both minimum surface oil or other thicker shell wall poses a stronger barrier against the fla-
entrapped constituent and maximum retention of the vor release as well as to the diffusion of oxygen and
core material inside the particle’s structure.[19] Quality moisture from the surrounding environment.[24] On
of the obtained product and the powder efficiency are the other hand, Paramita et al.[25] reported that the
dependent on the operating conditions such as inlet encapsulation efficiency of D-limonene is not signifi-
and outlet air temperature, feed temperature, and flow cantly dependent on the feed temperature.
rate as well as on the emulsion properties such as the
nature of oil phase, types of wall materials, ratio of wall
Inlet temperature
to core ingredients in the liquid dispersion, total solids
content, viscosity of the atomizing fluid, stability, and An appropriate adjustment of the air inlet temperature
droplet size.[20] 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
Feed temperature
before it comes into contact with the walls of the drying
Initially, feed temperature is one of the main factors that chamber. In a recent study, powders with higher con-
affect particle morphology and encapsulation efficiency. tent of bioactive compounds and higher antioxidant
In fact, feed temperature modifies the viscosity (fluidity) activity were produced at lower inlet drying tempera-
of the feed, its fluidity, and its capacity to be homoge- tures and higher feed rate.[27] The influence of dryer
neously sprayed. When the feed temperature increases inlet air temperatures has received considerable
to a certain level, viscosity and droplet size should attention.[28] Generally, it is desirable as the use of a
decrease but excessively high temperatures can cause high inlet air temperature to allow rapid formation of
volatilization or degradation of some heat-sensitive a semipermeable membrane on the droplet surface but
ingredients.[7] Shu et al.[21] who encapsulated lycopene yet not so high as to cause heat damage to the dry pro-
using a gelatin–sucrose system, reported that encapsula- duct or excessive bubble growth and surface disruption,
tion efficiency increased with an increasing feed tem- which increases losses during drying[29] or causes the
perature from 35 to 55°C, whereas when the particles to become sticky and cake.[30] For instance,
temperature was further increased to 65°C, the encapsu- the encapsulation efficiency of lycopene using malto-
lation efficiency decreased. Similarly, the encapsulation dextrin as wall material increased with an increasing
efficiency of lycopene using maltodextrin as wall inlet air temperature from 110 to 150°C, whereas when
material increased with an increasing feed temperature the temperature increased to 160°C, the efficiency
from 20 to 45°C, whereas when the temperature remained almost constant.[22] Similarly, increasing inlet
increased to 70°C, the efficiency decreased temperature from 170 to 210°C, the encapsulation
significantly.[22] This observation may be attributed to efficiency of lycopene increased with temperature at
the effect of feed temperature on emulsion viscosity. first, but then decreased dramatically when temperature
Brückner et al.[23] reported that the ideal feed tempera- reached the upper limit of 210°C.[21] In addition, micro-
ture for microencapsulation of food ingredients is 40°C encapsulation of vitamin C by spray drying, using gum
due to the lower feed viscosity and the higher drying arabic as a microencapsulating agent, was studied at dif-
rate, which leads to a quicker formation of the dry layer ferent air temperatures (140–200°C) and wall material
of carrier material around the droplet. On the other concentrations (10–20% aqueous solutions). The high-
hand, a feed temperature of 60°C was found to be dis- est concentrations of vitamin C were obtained on higher
advantageous, because it lowers the viscosity of the car- ranges of inlet air temperature, 152°C, and gum arabic
rier material, allowing for internal mixing inside the concentration, 18%.[31] Similarly, de Souza et al.[32]
particle during the drying process, thus retarding the reported that with increased temperature and lower car-
desired formation of a semipermeable crust around rier agent concentration (10%), there was a decrease in
the particle.[23] Furthermore, Yamamoto et al. investi- anthocyanin retention due to the degradation of these
gated the effect of feed temperature on encapsulation molecules. Therefore, the high air temperatures should
efficiency of D-limonene using a mixture of gum arabic accompanied with high solid concentration of solution
and maltodextrin. The results showed that the powder to achieve high encapsulation efficiency and
142 C. G. DROSOU ET AL.

preservation of the bioactives. Moreover, the influence the physicochemical properties of both wall and core
of inlet temperatures (160–200°C) on spray drying of materials used in a particular spray drying process.
mandarin oil was evaluated and an increase in inlet Higher core loads resulted in poorer retention or lower
air temperature favored the retention of the volatile encapsulation efficiency and a higher core material con-
oil.[33] Similar behavior was observed by Botrel et al.[8] tent at the surface of the powder particles.[56–58] This
and Fernandez et al.[34] in the microencapsulation of trend may be attributed to greater proportions of core
rosemary essential oil and fish oil by spray drying. It is materials close to the drying surface, thereby shortening
well known that an increase in inlet air temperature the diffusion path length at the air–particle interface.
(within limits) leads to the rapid formation of a semi- For instance, the encapsulation efficiency of lycopene
permeable membrane around the emulsion droplet, increased with an increasing core-to-wall material ratio
thereby providing better retention of volatiles.[35] On from 1:19 to 1:3, whereas when the ratio increased
the other hand, Paramita et al.[25] reported that increasing further to 1:1.5, the efficiency decreased. Minemoto
inlet air temperature from 120 to 150°C results in lower et al.[59] also observed that the encapsulation efficiency
flavor retention on spray-dried powder. These authors of linoleic acid decreased when the weight ratio of core
also reported that higher inlet air temperature promoted to wall material increased. According to these authors,
the vaporization of flavor during drying process. 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
Outlet temperature
efficiency. Moreover, Soottitantawat et al.[60] reported
The influence of dryer outlet air temperature on bioac- a significant increase in the surface oil of microencapsu-
tive retention is not well documented. Actually for a lated L-menthol when the mass ratio of L-menthol:wall
given spray dryer system, the outlet temperature material was increased from 1:9 to 3:7, using gum arabic
depends on the combination of inlet temperature and and two types of modified starch (Hi-Cap 100 and Cap-
feed rate. Lower outlet temperatures are reached with sul) as wall materials. In most of the published works, a
higher feed rate since the amount of liquid in contact typical core-to-wall material ratio of 1:4 was adopted
with the drying gas is higher and therefore higher quan- and identified as being optimal for various wall materi-
tities of heat are involved for moisture evaporation. als, such as gum arabic and modified starches.[19,61] In
Although higher temperatures promote faster evapor- another study, the encapsulation efficiency of pepper-
ation and a rapid crust formation, it is important to take mint oil decreased with an increase in the initial oil con-
into consideration the temperature of degradation of the centration from 70.6% for 10% oil to 57.2% for 30% oil,
materials to minimize losses of the bioactive using maltodextrin as wall material.[46] Similar behavior
compounds.[36–38] A recent work on the encapsulation was noted by Huynh et al.[39] and Tan et al.[57] in the
of lemon myrtle oil reported that the outlet air tempera- microencapsulation of lemon myrtle oil and fish oil by
ture of the spray dryer had little effect on oil retention spray drying. In another study, the influence of wall
but the surface oil increased significantly with the material concentration on the properties of rosemary
increasing outlet air temperatures, presumably due to oil microencapsulated by spray drying, with gum arabic
the temperature-mediated enhancement of oil as carrier was investigated. The results indicated that oil
diffusion.[39] Another study demonstrated that a higher retention was affected significantly (p < 0.05) by the
flavonoid content is obtained in the powder at an outlet wall material concentration and higher oil retention
drying temperature of 100°C than at 160°C.[27] In values were observed when there was a high solid con-
addition, encapsulation of bitter melon was conducted tent in the liquid dispersion compared with its low solid
by spray drying to optimize the inlet (125.6, 130, 140, content counterpart.[34]
150, and 154.1°C) and outlet (72.9, 75, 80, 85, and
87.1°C) temperatures of the process; optimal inlet and
Emulsion characteristics
outlet temperatures were 140 and 80°C, respectively.[40]
Table 1 summarizes the experimental conditions (inlet Another important factor in the microencapsulation of
and outlet temperature) for the encapsulation of differ- oils is the physical stability of the emulsions from which
ent food ingredients by spray drying. 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-
Core–wall material concentration
eral, emulsions with weaker stability result in encapsu-
There is an optimum concentration of core material lated powders with higher surface oil contents and a
that could be encapsulated efficiently depending on 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 used, gum arabic solutions are of relatively low viscosity
droplets results in greater retention of volatiles and even at high polymer concentrations On the other hand,
lower surface oil.[64–66] According to Jafari et al.,[19] proteins are surface active and have the ability to form
the higher surface oil in the particles produced from films at the interface and stabilize emulsion droplets;
emulsions with larger droplets can be attributed to as a result, in many studies, blends of carbohydrate
droplet breakdown during atomization. The reduction and proteins are being used.[8] In addition, the incor-
in size can be achieved, for example, using high-press- poration of hydrolyzed carbohydrates (maltodextrins,
ure homogenization or by increasing the emulsion vis- oligosaccharides) into the wall system has been shown
cosity or decreasing the oil load. For instance, in a to improve the drying properties of the wall matrix,
microencapsulation process of flaxseed oil by spray dry- probably by enhancing the formation of a dry crust
ing, lower oil content resulted in higher emulsion around the drying droplets and increasing the oxidative
viscosity.[67] Many authors reported that an increase stability due to reduced oxygen permeability.[73]
in emulsion viscosity generally reduces the time needed In recent decades, lipophilic bioactive components,
to form a semipermeable membrane or an outside shell such as oils and carotenoids, have been gaining great
in the atomized droplets at the early stages of the drying public interest globally due to their health benefits.
process.[19,39,60] According to Huynh et al.[39] and However, oils, containing a high amount of omega-3
Tonon et al.,[67] the membrane formed around the fatty acids, are highly susceptible to oxidation; oxidation
droplet surface becomes impermeable to larger com- of omega-3 fatty acids leads to peroxide formation and
pounds such as flavors and oils, thus reducing the oil finally to volatile compounds, some of which produce
migration to the particle surface. 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
Encapsulation of bioactive compounds by
and their incorporation into food systems or in food
spray drying
supplements has been extensively investigated by the
Spray drying is the most commonly used encapsulation food industries.[75] For instance, flaxseed oil, one of
technology in the food industry and is considered as a the richest sources of plant-derived omega-3 fatty acids,
cost-effective way to produce microcapsules in a rela- has been stabilized using microencapsulation by spray
tively simple and continuous processing operation.[68] drying and the results showed that whey proteins and
Since the main purposes of microencapsulation are to sodium caseinate improved the oxidative stability of
protect sensitive components in solid carriers, to reduce flaxseed oil during storage.[76] In another study, the
volatility, to promote easier handling, and to control the encapsulation of flaxseed oil using a mixture of
release of the encapsulated material during storage and maltodextrin with gum arabic or whey protein concen-
in applications,[69] the selection of an appropriate wall trate (WPC) or two types of modified starch (Hi-Cap
material is critical to the encapsulation efficiency by 100TM and Capsul TA) at a 25:75 ratio was investi-
spray drying.[70] Depending on the core material and gated; with respect to encapsulation efficiency, the blend
the characteristics desired in the final product, wall of maltodextrin:Hi-Cap showed the best performance,
materials can be selected from a wide variety of natural while the mixture of maltodextrin:WPC enhanced the
and synthetic polymers. Among the available ingredi- protection of the active material against oxidation upon
ents, the major wall materials used for spray drying storage.[47] In addition, flaxseed oil containing crawfish
applications are carbohydrates, including modified astaxanthin powder was successfully encapsulated by
and hydrolyzed starches, cellulose derivatives, gums spray drying using a wall system consisting of sodium
(exudates, extracts, etc.), and cyclodextrins as well as caseinate and lactose. The microencapsulation efficiency
proteins including whey proteins, caseinates, and for crawfish astaxanthin was 86.06%, which indicated
gelatin.[19] The wall material must be soluble in water that more oil was encapsulated than displaced on the
as almost all spray drying processes in the food industry particles’ surfaces.[77] Furthermore, Botrel et al. investi-
are conducted using an aqueous feed formulation as gated the encaspulation efficiency of fish oil using
well as should have film forming and good emulsifi- different blends of whey protein. The use of maltodex-
cation properties, and finally the wall concentrated trin or inulin together with whey protein is a good
solutions should be of low viscosity.[70,71] For instance, alternative in the spray drying process of fish oil as
carbohydrates, with the exception of gum arabic, lack the surface oil content was 5.6, 6.5, and 7.7% for the
active surface properties and must be used in conjunc- particles produced using whey protein:inulin, whey
tion with emulsifying agents to encapsulate hydro- protein:maltodextrin, and whey protein alone,
phobic core materials;[72] among the polysaccharides respectively.[70] Moreover, spray drying has been
DRYING TECHNOLOGY 145

successfully applied for carotenoid stability in oils such facilitates their incorporation into aqueous food systems
as gac oil which is rich in β-carotene and lycopene. as well as of possibly exerting health benefits (antioxi-
Specifically, gac oil was encapsulated using a mixture dant and anti-inflammatory effects). However, the food
of WPC and gum arabic at a ratio 7/3 (w/w), as opti- industry requires effective technologies which protect
mized in a previous study,[48] and the encapsulation the natural pigments, due to their instability under dif-
efficiency of the oil, β-carotene, lycopene was 87.22, ferent environmental stresses (light, air, humidity, and
82.76, and 84.29%, respectively under optimal con- high temperatures) and interactions with other food
ditions of inlet, 154°C, and outlet temperatures, constituents.[3] Currently, to accomplish this protection,
80°C.[78] In another study, maltodextrin was used to microencapsulation by spray drying is used by applying
produce gac powder by spray drying and the results different biopolymers as wall materials. For instance,
showed that total carotenoid content and antioxidant microencapsulation of anthocyanin pigments present
activity were preserved at inlet temperature of 120°C in Garcinia indica Choisy was performed with malto-
and maltodextrin concentration of 10%.[79] Addition- dextrins of various dextrose equivalents (DE 06, 19,
ally, encapsulation by spray drying is applied to oleore- 21, and 33) and other additives such as gum arabic
sins which are susceptible to degradation in the and tricalcium phosphate to enhance the stability of
presence of air, light, moisture, and high temperatures the pigment. The microencapsulated pigment using dis-
and have short storage life if not stored properly.[42] persions containing 5.0% maltodextrin DE 21, 0.25%
For instance, microencapsulation of cinnamon oleoresin gum arabic, and 0.25% tricalcium phosphate was found
by spray drying helps to stabilize oleoresin by prevent- to have the highest antioxidant activity (69.90%) and
ing against volatile losses. Gum arabic is considered to anthocyanin content (485 mg/100 g).[83] In another
be a better wall material for encapsulation of cinnamon study, the stability of anthocyanins and antioxidant
oleoresin as compared to maltodextrin, and modified activity of blackberry powder, obtained by spray drying,
starch, although the blend of gum arabic:maltodextrin: using maltodextrin, gum arabic, or a blend of both car-
modified starch (4:1:1) proved to be more efficient.[42] riers was studied. Maltodextrin provided greater stab-
The microencapsulation of garlic oleoresin by spray ility for spray-dried blackberry powder, because the
drying was investigated and the optimum conditions particles produced with this wall material exhibited
were found to be 10% garlic oleoresin, 60% maltodex- the longest half-life and the lowest anthocyanin degra-
trin concentration, and 200°C inlet air temperature, dation rate at 25°C.[84]
with maximum encapsulation efficiency of 81.9%.[80] Phenolic compounds have been also attracting con-
Furthermore, zein was used as coating material to siderable interest because of their positive effects on
encapsulate tomato oleoresin by spray drying and the human health. However, polyphenols show low water
results showed that zein particles could protect most solubility and low stability to different environmental
of the lycopene from being released in the stomach.[81] conditions (exposure to light, oxygen, temperature,
Similarly, essential oils are quite susceptible to oxidation and enzymatic activities). For these reasons, several
and volatilization and therefore are encapsulated to microencapsulation systems have been examined to
increase their shelf life and enable their controlled preserve the biochemical functionalities of these
release and the conversion of liquid flavorants into components.[85,86] For instance, Paini et al.[87] investi-
solids.[56] The microencapsulation of the essential oil gated the encapsulation efficiency of olive pomace poly-
from the fruits of Pterodon emarginatus by spray drying phenols and the highest total phenolic content was
using gum arabic and maltodextrin was studied. A obtained at inlet air temperature 130°C, maltodextrin
blend of 1:3:3.6 of oil:gum arabic:maltodextrin offered concentration 100 g/mL, and feed flow rate 10 mL/
the best protection, with 98.63% of the essential oil min. In addition, peanut sprout extract, rich in resvera-
being retained.[82] Spray drying microencapsulation of trol, was successfully encapsulated using WPC or malto-
Lippia sidoides essential oil was investigated using dextrin emulsions and the stability of capsules was
maltodextrin and gum arabic at different ratios. The investigated. The powdered peanut sprout extract
best encapsulation efficiency was achieved at maltodex- microcapsules coated with WPC exhibited high stability
trin:gum arabic ratio 0:1 and a carrier:essential oil ratio during storage, over 80% at 4 and 20°C during 10-day
of 4:1.[50] storage.[88] In another study, cinnamon polyphenols
Recently, there is an increased demand for food col- were encapsulated using maltodextrin as a wall material
orants from natural sources to substitute synthetic dyes. and the highest total phenolic content and antioxidant
For example, anthocyanins are considered as potential activity were observed at inlet temperatures of 160
replacements for synthetic colors because of their and 180°C and flow rate of 10 mL/min.[89] Finally,
bright, attractive hue, and water solubility, which 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.


DRYING TECHNOLOGY 147

the coaxial methodology, the polymer and the core noticed at higher concentrations of zein, while the
material are introduced into the electrohydrodynamic average diameter of the electrospun fibers
equipment from separated solutions; thus, the compo- increased.[92,104,107,108] In addition, b-cyclodextrin
nent immiscibility problem is alleviated.[97] (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-
Parameters influencing fiber characteristics in ined. The viscosity of b-CD/PVA solution increased
the electrospinning process with the concentration of b-CD and it was noted that
The electrohydrodynamic process has been attracting the high viscosity of b-CD/PVA solution led to forma-
considerable attention for the production of polymer tion of more uniform nanofibers with larger average
fibers or particles as it can generate them with diameters diameter. The same trend was observed for PVA/
in the range from several micrometers down to tens of chitosan blend nanofibers.[109] As far as molecular
nanometers.[98] It is well known that fiber or particle weight of the solubilized polymeric chains, Deitzel
diameter and morphology are strongly dependent on a et al.[100] and Geng et al.[110] showed that very low-
number of parameters.[90] These include intrinsic molecular weight polymers have a tendency to form
properties of the polymer solution such as type of poly- beads rather than fibers, whereas high-molecular weight
mer, conformation of the polymer chain, viscosity, elas- polymers give fibers with larger average diameter if the
ticity, electrical conductivity, polarity, and surface concentration of the polymer is adequate, presumably
tension of the liquid dispersion. Moreover, operational due to more extensive interchain associations.
conditions such as the strength of the applied electric
field, the distance between spinneret–collector and the Surface tension
feeding rate of the polymer solution are known to influ-
ence the fiber or particle characteristics. Other variables, The surface tension of a liquid dispersion, being a func-
such as the humidity and temperature of the surround- tion of composition (solvent and dissolved constituents)
ings may also play an important role in determining the and temperature, plays a critical role in the electrospin-
morphology and the diameter of the electrospun struc- ning process.[99] It is the primary counteracting force to
tures as well as their physical state.[92,99–103] The proces- the charge effects generated by the applied voltage dur-
sing parameters of electrohydrodynamic process are ing the electrospinning process and determines the
given in Table 2. overall electrospinnability of the liquid medium.[111]
Surfactants are often used for electrospinning fibers to
improve the electrospinnability, to reduce the electro-
Polymer concentration and solution viscosity spun fiber diameter, to eliminate the formation of
Initially, the solution viscosity is a critical factor that beaded fibers, and to form core–shell fibers by emulsion
influences solution spinnability and morphology of the electrospinning.[112] The influences of surfactants on the
electrospun fibers. Viscosity is directly related to con- diameter size and uniformity of electrospun poly(L-lac-
centration, molecular weight, and the structure and tic acid) fibers were examined by adding various surfac-
conformation of the polymeric chains as well as solvent tants (cationic, anionic, and nonionic), and significant
type.[104,105] Generally, an increase in viscosity increases diameter reduction and uniformity improvement were
fiber diameter and uniformity.[100,106] The effects of zein achieved in this way.[113] In addition, blend solutions
solution’s concentration and viscosity on electrospun of chitosan and poly(ethylene oxide) (PEO) at different
fiber morphology and size were investigated and the acidities and in the presence of surfactant Tween 20
authors report that beadless and uniform fibers were 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
Table 2. Processing parameters in electrohydrodynamic than the others. This was attributed to an increase in
processes.
acetic acid concentration that gave viscous solutions
Solution properties Viscosity
Polymer concentration with lower surface tension and an adequate polymer
Molecular weight of polymer chain entanglement.[114] On the other hand, the effect
Surface tension
Electrical conductivity of Tween 20 was neither a significant factor on fiber
Processing conditions Applied voltage diameter, while Wang et al.[112] have reported that the
Flow rate
Tip to collector distance
average diameter of the fibers decreased as the con-
Ambient conditions Temperature centration of the nonionic surfactant, TritonX-100,
Humidity increased.
148 C. G. DROSOU ET AL.

Conductivity cone and facilitate solvent evaporation.[99,123] The feed


rate therefore determines the amount of solution avail-
The electrical conductivity of solution also plays an
able for the electrospinning process. Typically, when the
important role on fiber morphology and size;[115] this
feed rate increases, a corresponding increase in the fiber
property is related to the charge density on a jet (liquid
diameter is observed.[124] Few studies have systemati-
stream), thereby affecting the extent of elongation of
cally investigated the relationship between solution flow
the jet by the applied electrical force. Under the same
rate on fiber morphology and size. For instance, Okutan
operating voltage and spinning distance, a solution with
et al.[111] investigated the influence of feed rate during
a higher electrical conductivity may cause higher elon-
electrospinning on properties of electrospun gelatin
gation of a jet along its axis and thus yield electrospin-
and reported that with the increasing feed rate, there
ning fibers of smaller diameter.[116] For instance, Tan
were larger fiber diameters and bead formations. More-
et al.[116] investigated the effect of solvent electrical
over, zein fibers were produced at 1.0 and 2.0 mL/h sol-
conductivity on morphology of electrospun poly
ution feed rate and the fiber diameters ranged from 250
(L-lactide-co-caprolactone) fibers using dichloro-
to 275 nm and from 250 to 350 nm, respectively.[122]
methane (DCM), N,N-dimethylformamide, and pyri-
Similarly, Henriques et al.[125] observed that the average
dine as solvents. The results showed that electrospun
diameter of electrospun PEO fibers increases linearly
polymer nanofibers with the smallest fiber diameter
with solution feed rate.
and highest uniformity were obtained from the DCM/
pyridine (50/50 wt%) solution, having the highest
electrical conductivity. The same trend was also noted Tip to collector distance
for poly(acrylic acid)[117] and polystyrene[118] fibers.
Another influential parameter is the distance between the
needle tip and the collector device, and this is correlated
Applied voltage with the flight time of the electrospinning jet. Longer
flight time may produce a thinner fiber as the fiber gets
The applied voltage is the critical element of any electro- more time to stretch and elongate before it is accumu-
spinning process because it provides surface charge on lated on the collector.[126] Consequently, the fiber diam-
the electrospinning jet, and thereby influences the nano- eter generally decreases with larger distance between
fiber diameter. Generally, increasing applied voltages needle tip and collector.[127] Nevertheless, Lee et al.[128]
lead to decreasing diameters of nanofibers due to have proposed that the fiber diameter increases at a
increasing electrostatic repulsive forces on the fluid jet,- longer distance due to reduction of the effective voltage.
[99,119]
e.g., for chitosan nanofibers produced by electro- Similarly, Sencadas et al.[120] instigated the influence of
spinning it was noted that by increasing the voltage, the the distance between the needle tip to the grounded
diameter of nanofibers decreased.[120] However, very collector on the fiber average diameter of a 7% (w/v) chit-
high voltages may facilitate nanofibers of larger dia- osan in 70/30 trifluoracetic acid (TFA)/DCM solution. It
meters as increasing the voltage above a certain level was observed that the fibers with the smallest average
increases the electrostatic stresses, which in turn, may diameter, ∼260 nm, were obtained for samples with
draw more material out of the syringe.[103,121] For 5 cm in distance between the needle tip and the collector
instance, zein solutions were electrospun at different and that the mean fiber diameter increased by increasing
applied voltages and the results showed that the low vol- the distance between the needle tip and the collector. A
tages gave small fiber diameters. Specifically, an applied maximum average fiber diameter of ∼500 nm was
voltage of 13 kV gave fiber diameters ranging from 250 obtained for a traveling distance of 20 cm.[120]
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 Humidity and temperature
high voltages.[100,121] 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
Flow rate
the influence of evaporation and solidification of the
The flow rate of the polymer from the syringe is another jet. Most investigations have been performed in an open
important process parameter as it influences the jet atmosphere without controlling the vapor concentration
velocity and the material transfer rate. A minimum of the solvent. Tripatanasuwan et al.[129] investigated the
value of solution volume suspended at the end of the effect of different relative humidity (5.1–63.5%) envir-
needle should be maintained to form a stable Taylor onments on PEO electrospun fiber morphology and
DRYING TECHNOLOGY 149

size. The average diameter of PEO nanofibers gradually increase in particle size with higher polymer concen-
decreased as the relative humidity increased. The evap- tration and viscosity has been also noted for other poly-
oration rate from the fluid jet decreased at higher rela- mers, such as polycaprolactone (PCL),[133] alginate,[134]
tive humidity, which allowed the charged jet to continue chitosan,[135] and elastin.[136]
to elongate. On the other hand, more beads appeared at
higher humidities.
Surface tension
Surface tension plays a role in the electrospraying pro-
Parameters influencing particle
cess, since it affects the ease of initial drop formation
characteristics in the electrospraying process
as the solution gets out of the nozzle. It is worth men-
The size and morphology of the particles prepared by tioning that the initial drops are formed when the elec-
electrospraying influence the release kinetics of the trostatic forces overcome the surface tension of the
entrapped bioactive compounds. Spherically shaped emerging liquid jet, and then these initial drops explode
particles are considered more suitable for delivery of to smaller drops as they travel in the electrostatic field
bioactives than irregularly shaped particles, mainly between the nozzle (usually positively charged) and
because of polymer dissolution and thus the bioactive the collector (usually negatively charged). A lower sur-
release might be inconsistent from within the irregularly face tension leads to smaller initial drops and hence
shaped particles.[130] Therefore, all the parameters that smaller final nanoparticles. The effect of higher surface
have an impact on particle morphology and size are tension on increased particle size has been reported for
discussed below. solutions of amylose and amylopectin[137,138] as well as
PCL.[139]
Polymer concentration, molecular weight, and
viscosity Conductivity
Polymer type, molecular weight, and concentration are The electrical conductivity of the polymer and solvent is
very influential factors in the electrospraying process; an important parameter when optimizing the electro-
i.e., changing polymer concentration and molecular spraying process as it affects the electrostatic attraction
weight largely affect the viscosity and surface tension of the charged particles to a grounded or oppositely
of the solution.[131] With greater length of polymer charged collector. With higher electrical conductivity,
chains, intermolecular associations are favored, parti- the Coulombian repulsion forces are enhanced and
cularly as the solution concentration is raised, leading compete with the viscoelastic forces of the solution; as
to larger size microcapsules. For low-molecular weight a result, disentanglements in the polymer chain network
polymers, a higher concentration is required for the for- occur during electrospraying, producing smaller parti-
mation of particles. In contrast, high-molecular weight cles. Gañán-Calvo et al.[140] showed that a decrease in
materials display a great number of entanglements, particle size can be obtained with an increasing solution
allowing particle formation even with polymer solutions conductivity. Nevertheless, if only conductivity had
of low concentration.[1] To have a stable process, it is been the parameter controlling the particle size, higher
important to take into consideration the viscosity of conductivity values would have produced larger particle
the polymer solution; with an increasing concentration, dispersity due to Coulomb fission forces, which over-
the increased viscosity leads to the production of cap- come chain entanglement forces, and thereby produce
sules with bigger size. For instance, Gomez-Estaca et al.[1] secondary droplets that are ejected from primary dro-
investigated the effect of zein concentration on the mor- plets, resulting in broader particle size distribution.[141]
phology of the resulting zein structures for polymer con- Correlating with viscosity, stable electrospraying can be
centrations ranging from 1 to 20% (w/w) in aqueous achieved only when viscosity is high or conductivity is
ethanol solutions. It was found that 1% of zein in the sol- low as reported for chitosan particles.[142] Changes in
ution was too low for particle formation, while a zein electrical conductivity can be obtained by changing
concentration of 20% gave rise to the transition from the electrospraying solvent or using cosolvents,
particles to fibers, a finding which was in accordance although this latter case may be detrimental to size dis-
with observations made in earlier work.[132] With zein tribution and morphology of the particles. For instance,
concentrations of 2.5 and 5% (w/w), the generated par- electrospraying was used to prepare poly(lactic-co-
ticles were round in shape and had relatively smooth glycolic acid) (PLGA) microparticles using two different
surfaces, whereas much larger particles in size were solvents, DCM and trifluoroethanol. Trifluoroethanol
obtained by increasing the polymer concentration. An enabled the preparation of even smaller sizes of PLGA
150 C. G. DROSOU ET AL.

particles, which can be attributed to the high conduc- Tip to collector distance
tivity of trifluoroethanol (TFE) (1.07 μS/cm) compared
Electrospraying distance can also affect capsules’ size
to DCM (0 μS/cm).[143] In addition, PLGA particles
and have an impact on the final product morphology.
were produced using a mixture of DCM with chloro-
In the electrospray process, once the compound jet is
form to increase the conductivity of the solution. The
formed, droplets are largely discharged by a needle con-
results showed that the addition of a solvent with high
nected to positive voltage. The position of the spray
conductivity destroys electrospraying stability and pro-
nozzle does affect particle size and particle size distri-
duces smaller and polydisperse particles. In another
bution. The investigation of this parameter revealed that
study, the effect of conductivity on particle formation
increasing the tip–collector distance decreases the aver-
was studied by adding the organic salt didodecyldi-
age size of particles as mentioned for amylose and
methylammonium bromide (DDAB) in the polymer
amylopectin[148] as well as for PCL.[139] This is due to
solution. The conductivity of a 5% (w/v) PLGA solution
the fact that a longer flight of droplets in the electric
in acetonitrile containing 10% (w/w) paclitaxel was
field, as a result of longer tip–collector distance, pro-
shown to increase from 0.51 to 116.5 μS/cm by the
vides more time for further coulomb explosions, and
addition of 2 mM DDAB. This led to a particle size
as a result smaller particles are being formed. In
decrease from around 1.2 µm to 355 nm.[133]
addition, increasing the distance leads to more spherical
morphologies since polymer chains have sufficient time
to diffuse within the droplet and thus also reduced
Applied voltage
polydispersity.[130] It must be pointed out, however, that
The applied voltage is a key parameter in achieving a increasing the tip–collector distance to more than a
stable cone-jet mode for obtaining monodispersed threshold will lead to disruption of drop breakage
nanoparticles.[1] Within the single cone-jet mode, size because of too weak electrical field.[148]
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 Blends of polymers used in
changed as stated by Shenoy et al.,[147] since as the volt- electrohydrodynamic process
age is increased, the particle morphology is largely
There has been growing interest in the development of
modified from a spherical shape to elongated particles
natural polymer-based nanofibers. Compared to nanofi-
or beaded fibers to eventually only fibers if the polymer
bers prepared from synthetic polymer solutions by elec-
concentration is sufficiently high. This is due to more
trospinning, bionanofibers have remarkable advantages
charge acting on droplets with increased voltage, lead-
in terms of high crystallinity, uniformity, biodegradabil-
ing to stretching and elongation of droplets. It is there-
ity, and biocompatibility.[149] However, electrospinning
fore recommended to use moderate voltages that allow
of nanofibers from biopolymers has proven to be quite
for the single cone-jet mode to take place while main-
challenging because these materials have limited solu-
taining the spherical morphology of the particles.[130]
bility in most organic solvents, are often polyelectrolytes
when dissolved, have poor molecular flexibilities, readily
form three-dimensional networks through hydrogen
Flow rate
bonding, and most importantly are insufficiently
The flow rate of the liquid stream in the electrospraying entangled to facilitate electrospinning.[150] Therefore,
process influences the size of the particles. Higher flow researchers have focused on the use of composite blends
rates could lead to a larger diameter of capsules as the of biopolymers with polymers that are compatible for
jet speed increases and higher concentration of polymer formation of electrospun fibers with enhanced material
solution drips out of the nozzle. Gomez-Estaca et al.[1] properties such as higher tensile strength.[151] Synthetic
noticed that the size of the particles decreased with polymers such as PEO and PVA, when combined with
the zein solution flow rate and the nanoparticle dia- biopolymers, improve the fiber forming ability of the
meters were observed to lie between 80 and 130 nm blending solution.[152] For instance, chitosan-based
and 130 and 175 nm for the 0.05 and 0.10 mL/h flow nanofibers have been successfully electrospun from
rate, respectively. The effect of the flow rate on the chitosan solutions blended with PEO,[153] PVA,[109,149]
diameter of several polymeric nanoparticles generated and silk fibroin.[154] Similarly, sodium alginate fibers
by electrospraying has been reported by several authors have been fabricated by electrospinning of aqueous mix-
using polymers such as PLGA,[144,146] chitosan,[135] tures in the presence of PVA[155–157] and PEO.[158,159] In
elastin,[136] and PCL.[133,139] addition, collagen was blended with PEO to produce
DRYING TECHNOLOGY 151

electrospun fibers.[160] In addition to synthetic poly- intermolecular and intramolecular forces, which need to
mers, there has been a lot of interest in the study of be somehow counteracted to promote capsule forma-
polymer blends, especially focused on biodegradable tion. In addition, the use of aqueous solutions further
and sustainable materials. Increasing attention has been complicates the process due to the ionization of water
given in recent years to natural polymers, such as poly- molecules at high voltages in an air environment, which
saccharides, due to their abundance in nature, unique may cause corona discharge. Moreover, aqueous solu-
structures, and characteristics with respect to synthetic tions present high-surface tension values which hinder
polymers.[161] This renaissance of polysaccharide mate- the formation of stable liquid fluid jets during the
rials is influenced by their useful properties including process.[166,167] One way to reduce the high surface ten-
nontoxicity, biocompatibility, biodegradability, and sion of aqueous solutions to stabilize the electrospraying
water solubility, making these biopolymers suitable for process is the use of surfactants. Surfactants are used in
different applications. Several polysaccharides, includ- a wide array of applications because of their potential to
ing starch, pectin, cellulose, chitin, and chitosan, have lower surface or interfacial tension of the medium in
been finding new potential uses in the food field. Chit- which they are dissolved.[168] For instance, capsules of
osan is the second most abundant biological polysac- low-molecular weight carbohydrates (e.g., maltodextrin,
charide (after cellulose) derived from nature and this resistant starch) were obtained by use of the surfactants
material finds many applications due to its unique Tween 20, Span 20, and lecithin.[169] In another study,
properties, such as antibacterial performance under cer- gums and surfactants were used to modify the aqueous
tain specific conditions.[162] Nevertheless, fiber forma- hydrocolloid dispersion properties allowing capsule for-
tion from chitosan by electrospinning on its own is mation through electrospraying. The results showed
rather difficult because of its limited solubility and poly- that the use of nonionic surfactants was the most inter-
cationic nature in solution. Therefore, Torres-Giner esting strategy for improving the sprayability of these
et al.[163] used blends of zein with chitosan to develop materials, since gums retained too much solvent that
novel antimicrobial materials which have potential for led to aggregated and wrinkled particles.[168]
applications in different fields such as active and bioac-
tive packaging, antimicrobial food coatings, etc.
Encapsulation of bioactive compounds by
Furthermore, zein nanofibers containing cyclodextrins
electrohydrodynamic process
(α-CD, b-CD, c-CD) were produced through electro-
spinning and the results showed that the addition of The growing consumer’s interest for the promotion of
cyclodextrin in the polymer solutions improves the elec- health and disease prevention through improved
trospinnability of the zein nanofibers at lower polymer nutrition has led to numerous attempts to develop
concentration. Thermal analyses showed that zein/ food-grade delivery systems, including active packaging,
b-CD nanofibers have higher glass transition tem- to encapsulate, protect, and controlled release of bioac-
peratures and higher degradation temperature with an tive components.[170–172] More specifically, natural
increasing cyclodextrin content. In another study, novel compounds with antimicrobial features are of great
ultrathin electrospun fibers from different blends of interest for the active packaging industry and their
amaranth protein isolate and the microbial polysacchar- efficient encapsulation and controlled release represent
ide pullulan were developed. The presence of pullulan a major challenge considering their sensitivity to heat,
(neutral polysaccharide with flexible conformation in oxygen, and light. Recently, electrospinning has been
aqueous solutions) in the blends resulted in increased receiving great attention in functional food and active
viscosity and lower conductivity of the solutions; these food packaging systems.[173,174] This relatively simple
led to improved chain entanglements and weakening technique can be applied for the production of nanofi-
of the polyelectrolyte character of the protein compo- brous polymeric membranes (coating films) formed by
nent, both favoring fiber formation.[164] Another work polymer fibers. Electrospun nanofibers exhibit proper-
described the electrospinning of zein/hyaluronic acid ties such as high porosity, large surface area per unit
blend fibrous membranes, where, to enhance compati- mass, high gas permeability, and small interfibrous pore
bility between the protein and the polysaccharide size, with most of these properties being quite important
components, poly(vinyl pyrrolidone) was introduced when these materials are used as carriers for delivery of
into the aqueous ethanol solutions of the blend.[165] bioactive compounds.[175,176] In the literature, few
The use of food hydrocolloids complicates the elec- works are focused on electrospinning of edible
trospraying process, since these materials may consist biopolymers,[132,177] and even less on edible polysac-
of low-molecular weight polymers which do not gener- charides for controlled release of bioactives. In general,
ate sufficient viscosity and they generally exhibit strong polysaccharides do not need toxic solvents to be
152 C. G. DROSOU ET AL.

electrospun[167] and are commonly used in food appli- immobilization of ( )-epigallocatechin gallate occurred
cations as coating and thickening agents, or additives when the fibers were aged for at least 24 h under dry
for technological aims. Common polysaccharide-based conditions at ambient temperature. Moomand and
wall materials used in electrospinning and electrospray- Lim[184] encapsulated fish oil, rich in omega-3 fatty
ing are pullulan, chitosan, alginates, dextrans, cellulose, acids, in zein fibers and the results indicated that electro-
and its derivatives. For instance, a blend of edible carbo- spun zein fibers provide a greater oxidative stability in
hydrate polymers (pullulan and cyclodextrin) was used comparison to nonencapsulated fish oil. These studies
to encapsulate antimicrobial aroma compounds for showed that electrostatic encapsulation processes are
enhancing microbial safety of food products. The very versatile for preparing a zein-encapsulant polymeric
release of aroma compound was negligible at ambient matrix to protect bioactive compounds. Furthermore,
conditions (23°C and 55% RH), even at high tempera- electrospun soy proteins have been used for controlled
tures (up to 230°C), but it occurs beyond a given relative release of allyl isothiocyanate.[185]
humidity threshold (90%),[178] presumably due to water On the other hand, electrospraying has been widely
plasticization of the carbohydrate matrix and the used to generate micro, submicro, and nanocapsules
underlying enhancement in molecular mobility of the for several applications in the area of encapsulation of
encapsulated components. In addition, folic acid has bioactive compounds.[186] Biopolymer-based particles
been encapsulated through electrospinning in amaranth are used to protect and deliver bioactive compounds
protein isolate:pullulan ultrathin fibers with very high in food systems or as fat replacers in foods by simulat-
encapsulation efficiency (>95%). Encapsulation within ing the rheological, optical, and sensorial properties of
the amaranth protein isolate:pullulan structures lipid droplets. For food applications, capsules are gener-
increased the thermal stability of folic acid and no degra- ally preferred rather than fibers, since apart from facil-
dation of it was observed after 2 h of UV exposure.[179] itating better handling and subsequent incorporation
Similarly, amaranth protein isolate:pullulan ultrathin into different products with minimal effects on sensorial
fibers were used to improve the antioxidant characteris- attributes, they usually present greater surface/volume
tics of two bioactive phenolic compounds, quercetin and ratio and, thus are expected to have better release pro-
ferulic acid, during an in vitro digestion protocol.[10] The files than fibers.[146] Therefore, there has been consider-
authors reported that the encapsulated bioactive com- able interest in the formation of biopolymer particles
pounds kept their antioxidant capacity to a greater from proteins and/or polysaccharides.[187] Recent
extent in comparison with the nonencapsulated ones works have demonstrated that it is possible to obtain
during in vitro digestion.[180] Moreover, other research- hydrocolloid-based encapsulation structures using elec-
ers have focused on the use of proteins as wall materials trospraying through proper adjustment of the process
for the encapsulation of active compounds. Common parameters and/or changing the solution properties
proteins used as encapsulating materials in electrospin- through the addition of proper additives.[168,169] For
ning are WPC, whey protein isolate (WPI), soy protein instance, WPC micro, submicro, and nanocapsules were
isolate, zein, gelatin, and casein. In this context, electro- produced through electrospraying from aqueous
spinning of zein (prolamine) shows an excellent outlook solutions for the encapsulation of the antioxidant β-
for its application in the stabilization of light and carotene. The results demonstrate that changes in pH
oxygen-sensitive food components;[181] zein is a hydro- of the solution have an impact on polymer confor-
phobic protein (prolamin) extracted from corngrains, mation and capsule size, with larger capsules being
and is known for its high thermal resistance and great obtained at pH 6.4. Moreover, the capsules were
oxygen barrier properties. Fernandez et al. (2009) effective in stabilizing the β-carotene against photo-
encapsulated β-carotene, a good source of provitamin oxidation as very high encapsulation efficiencies were
A with antioxidant properties, in ultrafine zein fibers achieved.[10] Electrospraying was also evaluated for the
through electrospinning and showed that the encapsu- encapsulation of folic acid using both a WPC matrix
lated β-carotene was stable and well dispersed within and a commercial preparation of resistant starch.
the zein fiber matrix. The electrospun β-carotene had Greater encapsulation efficiency was observed using
significantly higher light stability than the nonencapsu- WPC as wall material and the WPC protected the folic
lated control.[182] In addition, gallic acid had retained acid against degradation during storage, especially
its antioxidant activity after incorporation in zein under dry conditions. In another study, curcumin,
electrospun fibers.[183] Li et al.[132] encapsulated ( )- a food colorant with low solubility in water, was
epigallocatechin gallate in electrospun zein fiber to encapsulated in gelatin matrix, and the water solubility
stabilize the polyphenol during simulated food proces- and bioaccessibility were significantly improved by
sing conditions. The authors report that successful encapsulation.[188] Similarly, lycopene was encapsulated
DRYING TECHNOLOGY 153

through electrospraying within different edible biopoly- continuous production of dry powders and has been
meric matrices (dextran, WPC, and chitosan); it was widely used for the encapsulation over the past few dec-
seen that WPC presented the greatest encapsulation ades. However, in spite of the recent developments, the
efficiency (around 75%) and the WPC capsules were process remains far from completely being controlled.
also able to better protect lycopene against moisture In the spray drying process, the final properties of the
and thermal degradation.[189] Torres-Giner et al.[190] particles (e.g., size, size distribution, and morphology)
encapsulated docosahexaenoic acid (DHA) in zein cap- as well as the efficiency of encapsulation are affected
sules using an electrospraying process; the encapsulated by process parameters and solution properties; as a
DHA showed enhanced chemical stability against consequence, an extensive set of trial and error experi-
degradation under different environmental conditions ments are required for the production of microstruc-
such as relative humidity and temperature and reduced tures with desirable characteristics. Therefore, future
off-flavor notes. In another study, gelatin, WPC, and research needs to be focused on establishing a well-
soy protein isolate were compared as emulsion stabili- defined link between the solution properties, process
zers and wall matrices for encapsulation of a-linolenic parameters, and particle microstructure performance.
acid. The results showed that the WPC and soy protein Moreover, a great work remains to be made concerning
isolate capsules significantly delay the degradation of a- the choice of encapsulating materials according to the
linolenic acid at 80°C.[191] Extensive lists of applications chemical and physical nature of the core and wall
of electrospinning and electrospraying as techniques for material, the interaction (compatibility) between those
the encapsulation of bioactive compounds are presented as well as their relative proportion in the formulation
in Tables 3 and 4, respectively. of the capsules. In addition, the screening of new wall
biopolymers, which could ensure both the effective
preservation of functional components and the modu-
Future needs
lated release of the core ingredient, becomes essential
The food industry becomes more integrated with to replace overly used materials such as gum arabic
nutritional sciences due to current consumer demand and maltodextrins.
for natural and healthy products; therefore, it guides In recent years, electrospraying and electrospinning
and facilitates new processing approaches, including have attracted researchers’ interest due to their possible
encapsulation technologies, for the enrichment of food applications in food materials. These electrohydrody-
matrices with bioactive compounds. Generally, encap- namic processes have shown great potential for making
sulation has been used to protect bioactive compounds micro and nanosized particles and fibers and lately are
in food systems from adverse environmental factors and being used for encapsulating bioactive compounds.
to facilitate the control release at the targeted site. Spray Nevertheless, the potentialities of fibers and particles
drying is a well-established industrial process for the 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 Size range studied Purposes Reference
α-Linolenic acid Gelatin, WPC, and soy Nano-, submicro, and microcapsules Increase oxidative stability under thermal [191]
protein isolate were obtained treatment
β-Carotene WPC <100 nm Increase stability of the WPC capsules [10]
containing β-carotene against photo-
oxidation
Bovine serum albumin Poly(D,L-lactide-co- 3.0–5.5 µm Decrease the degradation rate of the [198]
glycolide) susceptible protein
Curcumin Zein 175–250 nm Enhanced stability and dispersion in aqueous [199]
food matrix
DHA Zein 500–700 nm Improve stability [190]
Ethylvanillin Ethylcellulose 45–85 nm Evaluate release profile of bioactive [200]
component
Folic acid WPC and commercial Nano, submicro, and microcapsules Increase stability of folic acid under different [201]
resistant starch were obtained conditions
Lycopene Dextran, WPC, and 0.8 ⌃ 0.3 µm (dextran), 2.1 ⌃ 0.7 µm Protect lycopene against moisture and [189]
chitosan (WPC), 0.2 ⌃ 0.1 µm (chitosan) thermal degradation
Maltol flavor Stearic acid/ethylcellulose 10–100 nm Limit flavor degradation or loss during [202]
processing and storage
WPC, whey protein concentrate; DHA, docosahexaenoic acid.

applications by the industry as more research is needed nozzles. Finally, despite the differences between the
to optimize the operating conditions and solution principles of both encapsulation techniques, several
properties for effective encapsulation of various bioac- common research needs can be identified, concerning
tives. For incorporation of such composite structures the improvement on encapsulation efficiency and
within food matrices, the use of food hydrocolloids as process optimization. In more detail, there is a need
encapsulating matrices is highly preferred, not only to enhance our understanding on interactions of core
for achieving a better integration of the capsules in and wall materials as well as on the relationships
the foodstuffs but also for improving consumer percep- between solution properties, process parameters, and
tion for these formulations. However, the use of biopo- functionality of the powder particles derived from these
lymers (e.g., natural food hydrocolloids) often two techniques. It is thus important to explore the rela-
complicates the electrohydrodynamic processes, due to tions between particle microstructure, dispersibility,
their poor viscoelastic behavior in solution, lack of suf- stability of the core material (upon storage in different
ficient molecular entanglements, and limited solubility; environments and under conditions encountered in
therefore, more research is needed to modify solution the gastrointestinal track), and controlled release
properties to enhance the spinning or spraying of food phenomena of the entrapped ingredients. As more
grade biopolymers. The selection of appropriate carriers information concerning structure–function relation-
needs to be further explored, in conjunction with the ships of such deliver systems becomes available, it
nature of the bioactive compound, so as to overcome would be feasible to produce tailor-made microcapsules
compatibility, stability, and bioavailability hurdles. for fortification of functional products with bioactive
Another complicating issue for the use of electrohydro- components.
dynamic processes is the multitude of optimizable fac-
tors. Only a few processing parameters can be
Conclusion
controlled directly as some of the parameters involved
are either highly interdependent or derive from the In this review, spray drying and electrohydrodynamic
properties of the used polymeric solutions. In addition, encapsulation technologies in food-related applications
a big challenge for such processes remains the scaling were discussed. The use of these technologies for the
for industrial purposes. Nowadays, these techniques encapsulation of food bioactive compounds aims to
have been successfully used on laboratory scale but their improve their stability and controlled release properties.
low throughput restricts their commercial exploitation The encapsulation efficiency, morphology, and micro-
at a larger scale. Specifically, the throughput of a single structure of the carrier structure are mainly affected
electrohydrodynamic setup is inherently low, owing to by the process parameters and polymer solution charac-
the relatively low flow rates adopted in the process, teristics. Although, spray drying has been a common
which are in the range of microliters per minute. One processing tool till now with a wide range of applica-
way to increase the production and simultaneously to tions in the food industry, the emerging electrohydrody-
compete with cost-effectiveness of the spray drying namic processes are gaining popularity lately due to
processes would be the development of an array of their high encapsulation efficiency and their ability to
DRYING TECHNOLOGY 155

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