A Project Submitted To

RAJIV GANDHI PROUDYOGIKI VISHWAVIDYALAYA BHOPAL

(M.P.)

2023-24

Partial Fulfillment of Requirement for the Project of Degree

BACHELOR OF PHARMACY
Submitted by
Hariom Patel
B pharma (7thsem)
(0605PY201031)
Under the supervision

Mr. Yogesh Sharma

(Associate Professor VIPER Sagar)
DEPARTMENT OF PHARMACY

VEDIC INSTITUTE OF PHAMACEUTICALS EDUCATION &

RESEARCH SAGAR (M.P.)

1
VEDIC INSTITUTE OF PHAMACEUTICAl EDUCATION &
RESEARCH, SAGAR (M.P.)
RAJIV GANDHI PROUDYOGIKI VISHWAVIDYALAYA BHOPAL
(M.P.)

2023-24

CERTIFICATE

This is certify that Hariom Patel student of B.Pharma 7th sem of VEDIC
INSTITUTE OF PHAMACEUTICALS EDUCATION & RESEARCH, SAGAR (M.P.)
has been completed his project on “Microencapsulation” to award the partial
fulfillment for the Degree Course In Pharmacy Of Rajive Gandhi Proudyogiki
Vishwavidyalaya Bhopal (M.P.)

FORWORDED BY
PRINCIPAL

Dr. A.K. Upadhyay

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VEDIC INSTITUTE OF PHAMACEUTICALS EDUCATION &
RESEARCH, SAGAR (M.P.)
RAJIV GANDHI PROUDYOGIKI VISHWAVIDYALAYA BHOPAL
(M.P.)

2023-24
ACKNOWLEDGEMENT
If you are thinking this is just my work. It is never one person’s work alone, and in my
case, so many people supported me in particular I would like to thanks: First and for most,
I would like to express my deepest sense of gratitude to Almightily God, My Father and
Mother whose abundance grace and mercy has enabled me to complete this project
successfully and giving me support to overcome all the problems.
My most thanks go to my guide Mr. Yogesh Sharma (Associate professor VIPER). It was
only because of his generous attitude, constant encouragement, working on this project
was one of the most rewarding experiences in my life his caring and parental attitude
always enlightened the way during my work I am always indebted to him.

I express my gratitude and respectful regards to Dr. A.K. Upadhyay, Principle of VIPER Sagar,
for his valuable contribution and facilities provided regarding my dissertation work.
I am strongly thankful to, Dr. Ajay Singh Thakur , Associate Professor VIPER for her support,
unremitting encouragement and science & Research center guidance thought my projects
work.
I am strongly thankful to Dr. Ram darshan Parashar, (Associate Professor), Mrs. Renu Singh
(Associate Professor) for his support, unremitting encouragement and his guidance.
Throughout my projects work.
The chain of my gratitude would be definitely incomplete if I would forget to thanks the
first cause of this chain Aristotle works.

Thanking You Hariom Patel

0605PY201031

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VEDIC INSTITUTE OF PHAMACEUTICALS EDUCATION &
RESEARCH, SAGAR (M.P.)

RAJIV GANDHI PROUDYOGIKI VISHWAVIDYALAYA BHOPAL

(M.P.)

DECLARTION

2023-24

I have by declare that the project work entitled “Microencapsulation” submitted

to the vedic institute of pharmaceutical education & research sagar (M.P.) is a
record of an own work done by me under guidence of
“Mr. Yogesh Sharma”
I Futher declare that this report is submitted in the partial fulfillment of the
requirement for the Degree of Bachelor of Pharmacy Curriculum for RGPV
BHOPAL. The result ambodied in this have not been submitted to any other
University or Institute for the award award of degree of pharmacy.

Student Name
Hariom Patel
0605PY201031

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Chapter titles page
no. no.

1. Introduction 6

2. Type 6

3. Method 7-16

4. Properties 17-22

5. Advantages 23

6. Disadvantages 23

7. Application 24

8. Conclusion 25

9. Reference 26-28

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Introduction
Microencapsulation is defined as a process of enclosing or enveloping solids, liquids or even
gases within second material with a continuous coating of polymeric materials yielding
microscopic particles (ranging from less than 1 micron to several hundred microns in size). In
this process, small discrete solid particles or small liquid droplets and dispersions are
surrounded and enclosed by applying thin coating for the purposes of providing environmental
protection and controlling the release characteristics or availability of coated active ingredients.
Microencapsulation process is widely employed to modify and delayed drug release form
different pharmaceutical dosage forms. The materials enclosed or enveloped within the
microcapsules are known as core materials or pay-load materials or nucleus, and the enclosing
materials are known as coating materials or wall material or shell or membrane.

Microparticles:
“Microparticles” refers to the particles having the diameter range of 1-1000 μm, irrespective
of the precise exterior and/or interior structures.
Microspheres:
“Microspheres” particularly refers to the spherically shaped microparticles within the broad
category of microparticles.
Microcapsules:
“Microcapsules” refers to microparticles having a core surrounded by the coat or wall
material(s) distinctly different from that of the core or pay-load or nucleus, which may be solid,
liquid, or even gas.
Microcapsules can be classified on three types
i). Mononuclear: Containing the shell around the core.
ii). Polynuclear: Having many cores enclosed with in shell.
iii). Matrix type: Distributed homogeneously into the shell material.

Fig. 1: Classification of microcapsules

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Methods of microencapsulation:

(a) Air suspension:

Microencapsulation by air suspension method consists of the dispersing of solids, particulate
core materials in a supporting air stream and the spray coating on the air suspended particles
(Fig. 2). Within the coating chamber, particulate core materials are suspended on an upward
moving air stream. The chamber design and its operating parameters influence a recirculating
flow of the particles through the coating-zone portion of the coating-chamber, where a coating
material is sprayed to the moving particles. During each pass through the coating-zone, the
core material receives a coat and this cyclic process is repeated depending on the purpose of
microencapsulation. The supporting air stream also serves to dry the product while it is being
encapsulated. The drying rate is directly related to the temperature of the supporting air stream
used.

Fig. 2: Air suspension method for microencapsulation

(b) Coacervation phase separation:

Microencapsulation by coacervation phase separation method consists of 3 steps:
i). Formation of 3 immiscible phases: a liquid manufacturing phase, a core material phase and
a coating material phase.

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ii). Deposition of the liquid polymer coating on the core material.
iii). Rigidizing the coating usually by thermal, cross linking or desolvation techniques to form
microcapsules.

The deposition of liquid polymer coating around the interface formed between the core material
and the liquid vehicle phase (Fig. 3). In many cases, physical or chemical changes in the coating
polymer solutions can be induced so that phase separation of the polymers will occur. Droplets
of concentrated polymer solutions will form and coalesce to yield a two phase liquidliquid
system. When the coating material is an immiscible polymer, it may be added directly. Also
monomers can be dissolved in the liquid vehicle phase and subsequently polymerized at
interface. Important equipments necessary for microencapsulation by coacervation phase
separation method are jacketed tanks with variable speed agitators.
Coacervation is a simple technique which involves formation of a homogeneous layer of the
polymeric wall material around the core material. This is achieved by altering the
physicochemical properties of the wall material by change in temperature, pH, or ionic
strength. Here, the core material and the wall material are mixed to form an immiscible
solution. Then, phase separation is carried out by changing the ionic strength, pH, or
temperature to form coacervates, which are tiny liquid droplets, consisting of polymer-rich
dense phase. These coacervates then surround the core material, forming the microcapsules.
Electrostatic interaction between two aqueous media is responsible for liquid to gel transition,
that is, ionic gelation, hence, leading to the formation of coacervates. This technique is basically
used for encapsulating hydrophilic molecules. Such coacervation, which involves only one
polymeric material is called simple coacervation. One example of such a polymer can be
sodium alginate. In simple coacervation, sodium alginate is dissolved in water and the active
compound that needs to be encapsulated, which is usually an oil, is mixed into it and the
emulsion formed is released in drops into a gel-forming media like calcium chloride. Ionic
interaction between sodium alginate and calcium chloride leads to formation of insoluble
polymers, calcium alginate. Several studies have been reported showing successful use of this
technique in microencapsulation. Sweet orange oil was encapsulated by Jun-xia et al. (2011)
by coacervation using soybean protein isolate (SPI) as the wall material. Coacervation can also
involve more than one polymer, then it is called complex coacervation. One common example
of complex coacervation includes polymers, gelatin, and alginate. Gelatin is solubilized in
water at an acidic pH for obtaining positive charges and alginate is soubilized in water

8
 separately at a basic pH to obtain negative charges. The active compound to be encapsulated is
mixed into the alginate solution and homogenized properly. This alginate phase is then mixed
intensively with the gelatin phase and the temperature is raised until chemical reaction between
alginate and gelatin starts. The active compound gets encapsulated by the formation of
polycationic-polyanionic insoluble polymer around it. Liu et al. (2010) used complex
coacervation method for encapsulation and stabilization of flaxeed oil. Here, gelatin and gum
Arabic, the two oppositely charged polymers were used as the wall materials and the deposition
of these coating materials around the core was initiated by changing the pH of the medium.
However, the use of this method is limited as it best works only within a certain pH range and
with certain electrolyte and colloidal solutions.

Fig. 3: Coacervation phase separation method for microencapsulation

(c) Pan coating:

For relatively large particles, which are greater than 600 µ in size, microencapsulation can be
done by pan coating method, which is being widely used in pharmaceutical industry for the
preparation of controlled release particulates. In this method, various spherical core materials,
such as nonpareil sugar seeds are coated with a variety of polymers (Fig. 4). In practice, the
coating is applied as a solution or as an atomized spray to the desired solid core material in the
coating pan. Generally, warm air is passed over the coated materials as the coatings are being
applied in the coating pans to remove the coating solvent. In some cases, the process of final
solvent removal is accomplished in the drying oven.

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 Fig. 4: Pan coating method for microencapsulation

(d) Fluidized-bed technology

Fluidized-bed technology method for microencapsulation is used for the encapsulation of solid
core materials, including liquids absorbed into porous solids. This microencapsulation method
is expansively employed to encapsulate pharmaceuticals. Solid particles to be encapsulated are
suspended on a jet of air and afterward, are covered by a spray of liquid coating material. The
capsules are traveled to an area where their shells are solidified by cooling or solvent
vaporization. The processes of suspending, spraying, and cooling are repeated until the
attainment of the desired thickness of the capsule-wall. This is known as Wurster process when
the spray nozzle is located at the bottom of the fluidized-bed of particles.

(e) Spray drying and spray congealing:

Spray drying and spray congealing methods of microencapsulation are almost similar in that
both the methods entail the dispersion of core material in a liquefied coating agent and spraying
or introducing the core coating mixture into some environmental condition, whereby relatively
rapid solidification of the coating is influenced (Fig. 5). The main difference inbetween these
two microencapsulation methods are the means by which the coating solidification is carried
out. In spray drying method, the coating solidification is influenced by the quick evaporation

10
of a solvent, in which the coating material is dissolved. In spray congealing method, the coating
solidification is accomplished by the thermal congealing of molten coating material or
solidifying a dissolved coating by introducing the coating core material mixture into a
nonsolvent. Removal of non-solvent or solvent from the coated product is often done by
sorption extraction or evaporation.
Spray drying is a technique in which a feed solution, which is a mixture of the core material
and the wall material is atomized and formed into a mist inside a chamber, where hot air is
applied to convert the mist into powder. Depending on various factors like the characteristics
of the feed solution and operating conditions, powder of varied particle size can be produced.
In spray drying, the core material, that is, the material of interest gets trapped in the dried
powder. Some of the advantages of this method: it can be used for different encapsulating
agents, it is economical, flexible, can be used for many different types of materials and can be
scaled up easily. Many studies have shown successful implementation of this technique in
encapsulation. Cardamom Oleoresin was encapsulated within a mixture of maltodextrin,
modified starch, and gum Arabic using spray drying and the results showed increased
protection of oleoresins (Krishnan et al., 2005). Bayram et al. (2005) reported successful
encapsulation of sumac flavor in sodium chloride using spray drying.

Although spray drying is one of the most extensively used methods for microencapsulation and
has many stated advantages also, some studies have portrayed certain drawbacks of the
technique. Fang et al. (2006) reported that when hot air is used as a drying medium for
encapsulation of omega-3 fatty acids, dried powder has particles with highly porous structure,
making the powder more prone to oxidation, thus, reducing the shelf life. Similar results were
reported by Kolanowski (2005), while developing spray dried fish oil powder. Thus, it can be
said that the same method can be effective for encapsulating one kind of material, while having
drawbacks for some other kind of materials.

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 Fig. 5: Spray drying method for microencapsulation

(f) Multiorific-centrifugation
Multiorific-centrifugation method for microencapsulation utilizes the centrifugal forces to hurl
a core particle trough an enveloping membrane. Various processing variables of
multiorificcentrifugation method include (i) rotational speed of the cylinder, (ii) flow rate of
the core and coating materials, and (iii) concentration, viscosity and surface tension of the core
material. The multiorifice-centrifugal method is capable for microencapsulating liquids and
solids of varied size ranges with diverse coating materials. The encapsulated product can be
supplied as slurry in the hardening media or as dry powder.

(g) Solvent Evaporation

Solvent evaporation method is appropriate for liquid manufacturing vehicle (O/W emulsion),
which is prepared by agitation of two immiscible liquids. The solvent evaporation method
involves dissolving microcapsule coating (polymer) in a volatile solvent, which is immiscible
with the liquid manufacturing vehicle phase. A core material (drug) to be microencapsulated is
dissolved or dispersed in the coating polymer solution. With agitation, the core–coating
material mixture is dispersed in the liquid manufacturing vehicle phase to obtain the
appropriate sized microcapsules. Agitation of system is continued until the solvent partitions
into the aqueous phase and is removed by evaporation. This process results in hardened
microcapsules. Several techniques can be used to achieve dispersion of the oil phase in the
continuous phase. The most common method is the use of a propeller style blade attached to a
variable speed motor.

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 Various process variables namely rate of solvent evaporation for the coating polymer(s),
temperature cycles and agitation rates influence the methods of forming dispersions. The most
important factors that should be considered for the preparation of microcapsules by solvent
evaporation method include choice of vehicle phase and solvent for the polymer coating, and
solvent recovery systems. The solvent evaporation method for microencapsulation is
applicable to a wide variety of liquid and solid core materials. The core materials may be either
water soluble or water insoluble materials. A variety of film forming polymers can be used as
coatings.

(h) Polymerization:
The polymerization method of microencapsulation is used to from protective microcapsule
coatings, in situ. The method involve the reaction of monomeric units positioned at the
interface existing in-between a core material and a continuous phase, wherein the core material
is dispersed. The continuous or core material supporting phase is usually a liquid or gas, and
therefore, the polymerization reaction occurs at the interfaces of liquid-liquid, liquid-gas, solid-
liquid, or solid-gas.

(i) Interfacial cross-linking

In interfacial cross-linking method of microencapsulation, the small bifunctional monomer
containing active hydrogen atoms is replaced by a biosourced polymer, like a protein. When
the reaction is performed at the interface of an emulsion, the acid chloride reacts with the
various functional groups of the protein, leading to the formation of a membrane. The
interfacial cross-linking method of microencapsulation is very versatile for pharmaceutical or
cosmetic applications.
Fluidized bed coating
Fluidized bed coating is an encapsulation method in which coating material is sprayed onto the
fluidized core material. Here, the core material is fluidized by application of air, onto which a
coating material is sprayed. Different fluidized bed coating methods are: (a) Top spray (b)
bottom spray, and (c) tangential spray. In this method of encapsulation, coating efficiency of
the wall material is dependent on various parameters like feed rate of the wall material,
atomization pressure of the nozzle, inlet air temperature, and velocity, etc. Coronel-Aguilera
& San Martín-González (2015) encapsulated spray dried beta carotene with hydroxypropyl
cellulose using fluidized bed coating. Here, temperature and feed rate of hydroxypropyl

13
cellulose was varied to determine how these factors effected the film forming ability of the
coating material and, hence, the stability of beta carotene during storage.

Extrusion
Extrusion technology for microencapsulation can be used for producing highly dense
microcapsules. To use this method, the core and the wall material should be immiscible. Here,
the core and the wall materials are passed in such a way that the wall material surrounds the
core and they are passed through concentric nozzles, thus, forming droplets containing the core
surrounded by the wall material. Then solidification is done either by cooling or using an
appropriate gelling bath wherein the droplets fall and solidify due to formation of complex.
The encapsulates formed using this method are relatively larger in size than formed using any
other method and also, this technology is useful with limited wall materials.

Emulsification
Encapsulation using emulsification technique is done by dispersing the core in an organic
solvent, containing the wall material. The dispersion is then emulsified in the oil or water, to
which emulsion stabilizer is added. Encapsulation of the core occurs by formation of a compact
polymer layer around it, by evaporation of the organic solvent. This is one of the frequently
used techniques of encapsulation as the procedures involved are very simple. This technique is
widely used for encapsulating enzymes and microorganisms. Song et al. (2013) reported
encapsulation of probiotics in alginate-chitosan using emulsification and demonstrated better
resistance of the probiotics under stimulated gastrointestinal conditions.

Cyclodextrin inclusion
Cyclodextrins are cyclic oligosaccharides, capable of forming inclusion complexes with many
organic compounds. Cyclodextrins have an internal nonpolar cavity and hydroxyl groups on
the surface. Formation of inclusion complexes of cylodextrins with the hydrophobic
compounds mainly takes place by the hydrophobic interaction between the cyclodextrin surface
and the guest compounds. However, other forces, such as dipole-dipole interactions and van
der walls forces, may also be involved in the formation of the complexes (Rakmai et al., 2018).
There are several methods for obtaining inclusion complexes with cyclodextrin. Some of them
are: (a) Coprecipitation method, which is used for the nonwater-soluble substances. In this
method, the compound to be encapsulated is dissolved in organic solvents like benzene,

14
chloroform, diethyl ether, etc. and to this solution, cyclodextrin dissolved in water is added in
appropriate amount with proper agitation. The solution is then cooled for obtaining the complex
crystals. Finally, the crystals are washed using an organic solvent and dried. (b) Freeze drying
or lyophilization: this method is mostly used for thermolabile compounds. Appropriate amount
of cyclodextrin and the compound of interest are dissolved in water by proper stirring.
The solution is then freeze dried and the powder obtained is washed with an organic solvent
and dried under vacuum. (c) Spray drying: this method is used only for the thermostable
molecules. Cyclodextrin and the compound to be encapsulated are dissolved in deionized
water. And the solution is dried in a spray dryer.
In many food-related applications, cyclodextrins are used for encapsulation of flavor
compounds, as they provide better retention, protection, and enhance controlled release. Furuta
et al. (2008) explained in detail, the entrapment of food flavors in cyclodextrins, using freeze
drying and spray drying.
Different modified cyclodextrins, namely 2-hydroxypropyl-β-cyclodextrin, randomly
methylated β-cyclodextrin and triacetyl β-cyclodextrin were used for the inclusion of flavors,
namely, d-limonene, allyl isothiocyanate, and l-menthol. Inclusion of flavors in cyclodextrin
was done by preparing solutions, which were then spray dried or freeze dried. Depending on
the solubility of the cyclodextrin, different mediums were used for encapsulation.

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16
DIFFERENT PROPERTIES OF THE CAPSULES
Physical properties
Particle size and morphology of microcapsules
The particle size of the microcapsules depends on the different techniques which are used to
produce the microcapsules. Table 3 shows the variation in the particle sizes due to different
techniques used. Morphology of the microcapsules refers to the internal as well as the external
structure of the capsules which largely depend on the operating conditions that are used to
produce the microcapsules as well as the wall materials used. Different types of capsules can
be obtained—simple sphere surrounded by the wall material, capsules with irregular core,
multiple distinct cores within a continuous coating of wall material, multiwalled microcapsules
and core particles embedded within the matrix of wall material.
Porosity
Porosity of the microcapsules, formed using any technique, is one of the most important
properties of the microcapsules, responsible for their function in a particular food matrix. And
this property is greatly dependent on the composition of the wall material of the microcapsule
and the technique which is used to produce the microcapsule. Wall matrix, which holds the
core is designed in such a way so as to direct the mass transfer between the environment and
core (Rosenberg et al., 1985; Jackson & Lee, 1991; Shahidi & Han, 1993). The porosity of the
wall material plays a great role in controlling the permeation of volatiles within the capsule
(Arshady, 1993; Dziezak, 1988). It also determines the oxidative stability of the core of the
microcapsule by controlling the permeation of oxygen through it. In case of volatile cores, wall
permeability is a major factor for increasing the chances of core loss during storage (Rosenberg
et al., 1985). Moreau and Rosenberg (1999) examined the porosity of the spray-dried
microcapsules, encapsulating anhydrous milk fat within the mixture of lactose and whey
protein as wall system by using gas displacement pycnometry. In this study, helium and
nitrogen were used as the permeating gases. Results showed the differences in the way of
penetration of helium and nitrogen through the microcapsules. It was seen that helium could
fill all the accessible volume very fast, while penetration of nitrogen was comparatively slower.
Overall, the results of gas-displacement pycnometry indicated the presence of pores
characterizing both, anhydrous milk fat containing and core-free microcapsules (Rosenberg et
al., 1985). The microcapsules containing milk fat were found to be more porous than the ones,
which were free from the core material. Similar characteristics were obtained for the
microcapsules encapsulating fish oil with dextrin and sodium caseinate wall materials. Those
microcapsules also exhibited molecular-sieve kind of porosity, that is, with pores, which are
minute enough to prevent the entry of molecules. Likewise, Allan-Wojtas et al. (2008) also
reported the study of calcium alginate microcapsules, encapsulating probiotic bacteria. For
studying the microstructure of the capsules, cryo-Scanning Electron Microscopy (cryo-SEM)
and Transmission Electron Microscopy (TEM) were used. SEM results revealed the differences
between the structure of bacteria containing and the core-free capsules. The bacteria containing
capsules were found to be more porous as compared to the core free capsules, hence attributing
to the fact that the bacteria interfered with the formation of cross linking of the alginate with
calcium chloride, as described by Truelstrup Hansen et al. (2002) and Sultana et al. (2000).
TEM analysis also showed the similar results. Hence, for determining the porosity of
microcapsules, gas displacement pycnometry and electron microscopy, both can prove to be

17
very important tools for analyzing the microstructure of the capsules, useful for designing the
carrier substances for a particular core material.

Surface hydrophobicity
Surface hydrophobicity can be defined as a physical property of a molecule that is repelled by
water. This is a property which is largely based on the core material to be encapsulated and the
wall material. In a study by Mendanha et al. (2009), microcapsules were produced
encapsulating casein hydrolysate within SPI and pectin, the results showed that hydrophobicity
decreased with the increase in the concentration of casein hydrolysate in the formulation of the
microcapsule. With the increase in casein concentration, more and more hydrophobic
interactions were formed with SPI, thus, leading to the turning of the hydrophobic groups from
SPI to the core of the capsules, which in turn causes reduction in hydrophobicity. In another
study by Beaulieu det al. (2002) and Floury, Desrumaux et al. (2002), it was found that globular
proteins like soy and whey protein, which were used as wall materials, formed soluble
aggregates through surface hydrophobic interactions after high pressure treatment. Hence, it
can be seen that surface hydrophobicity is a very critical physical parameter which needs to be
considered, while selecting the shell material for encapsulation, as shell material properties
have a huge impact on the hydrophobicity of the microcapsules.

Flow properties
Flow properties of the microencapsulated powders include bulk density, tapped density,
porosity, and compressibility. Analysis of bulk density and tapped density of the capsules is
important in order to obtain the capacity of the powder formed, in packaging, storage, and the
distribution process. Bulk density is dependent on the particle density, size, shape, and water
content of the microcapsule (Shamaei et al., 2017), which in turn depends on the coating
material and technique used for encapsulation. Dependence of bulk density on the coating
material has been explained by Mehyar et al. (2014) in a study, where cardamom essential oil
was encapsulated using whey protein isolate (WPI), guar gum and carrageenan by freeze
drying. Bulk density of the microcapsules was highest when WPI was used alone as the coating
material as compared to combination of WPI with guar gum and carrageen. In a study by
Hermanto et al. (2016), bulk density of cinnamon oil microcapsule, encapsulated within a
coating of maltodextrin and gum arabic at different concentrations, was measured using a very
common method of tapping, which is also reported in Chinta et al. (2009). And it was found
that if the size of the microcapsule formed is small, it would lead to larger mass density of the
capsule due to decrease in the cavities between the particles. Also, higher levels of water leads
to increase in the weight of the material in the container, volume remaining the same, thus,
causing an elevation in the bulk density (Prabowo, 2010). Dependence of bulk density on the
technique used can be observed from the results reported by Shame et al. (2017). Herein, walnut
oil was microencapsulated using spray drying technique and the results revealed that with the
decrease in feed atomization pressure and increase in the inlet air temperature, the bulk density
of the microcapsules decreased. This was because, with the increase in inlet air temperature,
microcapsules with hollow structure and high sphericity were formed. Similar results were also
reported by Tonon et al. (2011).

18
Flowability of microencapsulated powder formed is determined by using two parameters,
percent compressability or Carr's Index and the Hausner Ratio (HR), as reported by Turchiuli
et al. (2005). Similar methods were adopted by Xue et al. (2013) for determining the flowability
of the lycopene microcapsules. The higher value of HR attributed to the fact that the powder
was cohesive, indicating high powder viscosity and was restricted to free-flow. Flowability
largely depends on the particle size and particle size distribution of the microcapsules, which
in turn is influenced by other factors like shape and surface roughness of the microcapsules.
Thus, it is very crucial to choose a particular wall material and a particular technique of
encapsulation to obtain the flow properties of the capsules as desired.

Micromechanical properties
Mechanical trigger of the microcapsules depends upon their micromechanical properties. It is
a fundamental need to study the mechanical properties of the microcapsules once they are
produced, so as to ensure that the release of the core material takes place at a specific target
and at a specific time and not before that. More specifically in many food applications, a very
adjustable kind of mechanical strength is desired in the microcapsules. The mechanical
properties of the microcapsules include elastic modulus, rupturing force that is required to
rupture the capsule and nominal rupture stress, which is equal to the rupture force divided by
the initial cross-sectional area of the microcapsule (Sagis, 2015). And these largely depend on
the core to shell ratio in capsule and also on the preparation and processing conditions, for
instance, different polymerization temperatures and time and difference in the drying methods
like oven drying, spray drying, or fluidized bed drying. The mechanical properties of the
microcapsules also depend upon the type of capsules formed, like whether they are multiwalled
or single-walled type. For example, there is this new technique called layer-by-layer(LBL)
deposition of the shell material, which involves adsorption of different biopolymers like
polysaccharide and certain protein fibrils in alternate layers, wherein the former is flexible and
the latter is stiff, leading to properties of the capsules, which are application specific. In such a
technique, mechanical strength of the capsules depend on the number of layers adsorbed and
also on the flexibility and rigidity of the biopolymers. Numerous methods for characterizing
the mechanical properties of the microcapsules made up of polymeric materials are evolving,
so the first task which comes in here is to find out the potential as well as the limits of different
techniques.

The methods for determining the mechanical properties of the shell are either tested on the
microcapsule itself or on the macroscopic surfaces. The methods for characterizing the
macroscopic surfaces, that is, microcapsule population, include compression between the
plates and the osmotic pressure test. Whereas methods for characterization of single
microcapsules include Atomic Force Microscopy, micropipette aspiration, and
micromanipulation. Some of these methods are discussed in the following section.
Colloidal foam Atomic Force Microscopy (AFM)
Colloidal foam Atomic Force Microscopy (AFM) method basically involves
microcompression of a single particle (Sagis, 2015). Herein, the capsule under consideration is
allowed to adsorb onto a substrate, which is then deformed by a colloidal probe particle
attached to a cantilever AFM, as shown in Figure 3. The probe particle compresses the
19
microcapsule by itself getting displaced in a vertical direction over a distance d. The force
required for displacement of the probe particle over a distance d can be calculated from the
known force constant of the cantilever and the deflection it undergoes, which is determined by
a laser.

Fluid-mechanics-based determination of mechanical properties

Microcompression of a single capsule: (a) probe centered above the capsule; (b) probe
displaced; (c) probe getting displaced leading to buckling of the shell
Mechanical properties of the microcapsules can be determined by applying extensional and
shear force on them in flowing fluid (Sagis, 2015). Rotating shear devices are used for this
purpose, as shown in Figure 4. These rotating shear devices have transparent concentric
cylinders with narrow gap between them, in which a very dilute dispersion of the microcapsules
is being poured. The microcapsules in the dispersion are deformed in such a way that they form
an angle with the flow direction, once the dispersion gets exposed to a steady shear field. The
degree of deformation as well as the orientation of the microcapsules gives their mechanical
characterization.
Osmotic swelling method
Rotating shear cell
For microcapsules having water permeable shell and aqueous core, their mechanical
characterization can be done by using this method (Sagis, 2015). In this method, the
microcapsules are made to come in contact with an aqueous high molecular weight polymer
with a continuous phase. Difference in osmotic pressure between the interior and the exterior
phase is created due to difference in the chemical potential of water between the two phases.
And when the concentration of the external polymer is very high, migration of water starts
taking place from the interior aqueous phase to the exterior one, until equal chemical potential
is reached on both the sides. As a result of this movement of water, there is a shrinkage in the
capsule, leading to the crumpling of the shell, as shown in Figure 5. In order to observe such a
phenomena, laser microscopy is used. The critical osmotic pressure required for crumpling is
determined and the shell characterization is done by plotting this critical pressure versus the
wall thickness of capsule.

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Method based on thermal expansion
Osmotic collapse of the microcapsule: (a) core moving out, (b) collapsed capsule
This method is used for mechanical characterization of the microcapsules with an oily core. It
is valid only when the coefficient of thermal expansion of the core material is more than that
of the shell material as well as the continuous phase in which the capsules are dispersed. In this
technique, capsules are dispersed in a continuous phase and they are observed under a
microscope with a thermal stage. The dispersion is subjected to a temperature that is
continuously increasing at a fixed rate. The core of the capsule expands more than that of the
shell and the continuous phase, which leads to the building up of stress inside the capsule. This
continues until the shells burst. This process is shown in Figure 6. Once the 90% of the capsules
are burst, temperature as well as the time required for bursting is recorded. Use of this technique
is reported by Humblet-Hua, van der Linden, and Sagis (2012) for shell characterization of the
microcapsules having shells reinforced with lysozyme fibrils, which were produced by using
LBL adsorption. No such studies have been reported in the food microcapsules.
Thermal expansion of microcapsules
Thermal properties
Thermal properties of microcapsules is one of the crucial properties to be studied so as to
determine their storage stability as well as the release rates. These can be obtained by a
technique called Differential Scanning Colorimetry (DSC). In this technique, there are separate
holders for sample and a reference in the instrument. Heaters are present which either increase
the temperature at a specified rate or holds the colorimeter at a given temperature. The
instrument measures the heat flow difference between the reference and the sample. Xie et al.
(2010) studied the thermal properties of the microcapsules encapsulating vitamin A within
starch octenyl succinate using DSC. From the DSC curve, an endothermic transition was
observed which attributed to the glass transition. The glass transition temperature (Tg) of the
microcapsule from the DSC thermogram was seen to be 56.355°C with the specific heat of
0.377 J/g. Tg value has a relation to the amorphous structure, which suggests that, at Tg value,
a substance changes its state from glassy to rubbery substance (Lim, Chang, & Chung, 2001;
Xie et al., 2010). Below the Tg value, the movement of molecular chain segments was found
to be poor, which indicated better protection ability to the core material. Tg value being
56.355°C, was greater than the normal storage temperature (25°C), which indicated good

21
storage stability of vitamin A microcapsules when stored at room temperature in a glassy state.
Thus, DSC results revealed that the glass transition temperature (Tg) and the melting
temperature (Tm) were 56.355 and 208.300°C, respectively, which showed that the vitamin A
microcapsules had the storage and heating stability. It can be clearly observed from the above
mentioned study that determination of thermal properties of the capsules is crucial for
indication of correct storage temperature and also the indication of the temperature at which
the food containing the microcapsules needs to be processed.

Functional properties
In addition to the physical, mechanical, and thermal properties of the microcapsules, functional
properties are also very important, especially while using the microcapsules to develop a new
product with added functional properties. Following are some of the important functional
properties of the capsules.

22
Advantages of microencapsulation:
i). Providing environmental protection to the encapsulated active agents or core materials.
ii). Liquids and gases can be changed into solid particles in the form of microcapsules.
iii). Surface as well as colloidal characteristics of various active agents can be changed.
iv). modify and delayed drug release form different pharmaceutical dosage forms
v). Formulation of sustained controlled release dosage forms can be done by modifying or
delaying release of encapsulated active agents or core materials.

Disadvantages of microencapsulation:
i). Expensive techniques.
ii). This causes reduction in shelf-life of hygroscopic agents.
iii). Microencapsulation coating may not be uniform and this can influence the release of
encapsulated materials.

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Applications:
Different applications of microencapsulation are:
1. Microencapsulation can be used to formulate various sustained controlled release
dosage forms by modifying or delaying release of encapsulated active agents or core
materials.
2. Microencapsulation can also be employed to formulate enteric-coated dosage forms, so
that the drugs will be selectively absorbed in the intestine rather than the stomach.
3. Gastric irritant drugs are being microencapsulated to reduce the chances of gastric
irritation.
4. The taste of bitter drug candidates can be masked by employing microencapsulation
techniques.
5. Through microencapsulation, liquids and gases can be changed into solid particles in
the form of microcapsules.
6. Microencapsulation can employed to aid in the addition of oily medicines to tableted
dosage forms to overcome the problems of tacky granulations and in direct
compression.
7. Microencapsulation can be used to decrease the volatility. A microencapsulated volatile
substance can be stored for longer times without any substantial evaporation.
8. Microencapsulation provides environmental protection to the encapsulated active
agents from various environmental issues, such as light, heat, humidity, oxidation, etc.
9. The hygroscopic characteristics of many core materials can be reduced by
microencapsulation.
10. The separations of incompatible substances can be achieved by microencapsulation. For
example, pharmaceutical eutectics can be separated by microencapsulation. This is a
case where direct contact of materials brings about liquid formation. The stability
enhancement of incompatible aspirin-chlorpheniramine maleate mixture is
accomplished by microencapsulating both of them before mixing.
11. Microencapsulation is used to lessen the potential danger of toxic substance handling.
The toxicity owing to handling of herbicides, insecticides, pesticides and fumigants,
etc., can be usefully lessened after microencapsulation.

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Conclusions

Microencapsulation as a delivery system has proved itself useful in a variety of commercial

applications in many areas of industry. The techniques used to produce these capsules range
from simple blend operations to complex polymeric coating systems. The systems discussed in
this chapter provide only a brief introduction to the world of microencapsulation and its
potential applications. It would be extremely difficult to list all the potential applications for
encapsulation systems as the list would be vast, but it can be summarized by the following
statement.

“The applications of microencapsulation are only limited to the creativity of the individual
formulator, and the experience of the encapsulation scientist.”

It is only through a joint effort between the formulating company and the microencapsulation
experts that an effective solution can be created to solve specific problems within any given
formulation.

The field of cosmetic science holds a bright future for the use of microencapsulation as a
delivery system for useful personal care actives. The personal care industry has seen a recent
surge in the use of active compounds used to treat skin deficiencies rather than simply masking
the problem. As the need for more active compounds increase, the formulation problems
increase in proportion to this need. It is a scientific fact that the more active the compound, the
more reactive it becomes with the environment in which the compound is placed. This is
especially true with respect to typical cosmetic formulations that can be considered harsh
environments for active compounds. It is in this arena that the microencapsulation techniques
can solve resulting stability issues and deliver the material in an active state to treat the problem
areas.

Features and benefits of using microencapsulation to enhance personal care formulations

include improving aesthetics, protecting the encapsulated compound, improving stability and
increasing the shelf life of the finished product, preventing incompatibilities within the formula,
controlling the release of the encapsulated compound, and assisting in formulating color
cosmetics.

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