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Emulsion

Mr. Pankaj Kusum Ramdas


Khuspe
Emulsion
 Introduction.
 Definition.
 Advantages and Disadvantages
 Classification of Emulsion.
 Theory of Emulsification.
 Formulation.
 Method of preparation.
 Evaluation of Emulsion.
Question bank
 Describe dry gum method (3.5).
 Describe any two test for identification of emulsion(3.5).
 Define creaming, How creaming of emulsion is minimized.
(3.5)
 What are emulgents, classify them.(2)
 Most of emulsion appear white. Why(2).
 Define emulsion.(2).
 Enlist the stability parameter for emulsion and describe
one.(3.5).
 Define emulsion, classify with emulsifying with example.
(3.5)
 What do you mean by creaming & cracking, enumerate
factors responsible for cracking.(3.5)
Introduction
emulsion originate from latin word
“emulgere” which means milk.
 It is a heterogeneous and biphasic

system.
Physical chemist:
 Thermodynamically unstable mixture.
Product development technologist:
 Intimate mixture of two immiscible liquid that
exhibit an acceptable shelf life near room
temperature.
Definition

 a biphasic liquid preparation


 containing two immiscible liquids

 which are made miscible

 by adding emulsifying agent


Definition

“EMULSION is a biphasic liquid preparation


containing two immiscible liquids which
are made miscible by adding emulsifying
agent”
EMULSION

 One of which is dispersed as minute


globules in to the other.
 The liquid which is converted
a. in to minute globules is called the

“Dispersed Phase” &


b. the liquid in which the globules are
dispersed is called the
“Continuous Phase”.
Advantages
1. Mask the Unpleasant taste.
2. Economical.
3. Improved Bio-availability.
4. Sustained Release Medication.
5. Nutritional supplement.
6. Diagnostic purpose (x-rays examination).
7. External use preparation
(cream lotion foam aerosol).
Disadvantages

 Short shelf-life.
 Unstable:- soluble phase separate

slowly
 Handling

 Storage.
Classification
a. According to emulsifying agent
containing:
 Natural product: polysaccharides, cellulose.
 Sterol/soap substances.
 Saponins.
 Starch.
 Natural wax.
 Surface active agent.
• Anionic surfactants
• Non-ionic surfactant
Classification

b. According to mode of administration:


 Oral: caster oil, liquid paraffin.
 External: o/w or w/o of emulsion.
 Parenteral: Vitamins,
 Rectal: enema.
Classification
c. According to Types of emulsion:
 Common emulsion:
 o/w:
 w/o:
 Multiple emulsion:
Use for subcutaneous and Intravenous injection.
 o/w/o
 w/o/w

 Macro emulsion: (0.1µm – 5µm)


 Micro emulsion/
micellar emulsion: (5µm – 140
nm)
Theory of emulsification

DROPLET STABILIZATION
1. Reduction in Interfacial Tension:
 Thermodynamically stabilization
1. Formation of Interfacial Rigid Film:
 Mechanical barrier to coalescence
1. Formation of Electrical Double
Layer:
 Electrical barrier to approach of particles.
Theory of emulsification
 Interfacial Tension:
 tension exist at interface of two
immiscible liquid
 stronger attractive forces for a molecule
at the interface.
 Surfactants are added to reduce
interfacial tension.
 Surfactant are absorbed at surface of
liquid and diminishes attractive force.
Theory of emulsification
Interfacial film formation (oriented-wedge
theory micelle formation):
 Emulsifying agent surrounding the droplet
of internal phase form a thin film adsorbed
at surface of droplet.
 Ampihillic EA: Hydrophilic (polar) end
absorbed in water phase and
hydrophobic/lipophilic (non-polar) in oil
phase.
 This prevent the coalescence of droplets.
Theory of emulsification

Oriented-wedge theory:
 There are three type of films formed:
 Monomolecular: Surface active agent,
anionic emulsifying agent, soaps.
 Multimolecular: Non ionic emulsifier,
polysaccharide (gums).
 Solid particle film: Inorganic emulsifying
agent
Theory of emulsification

Electrical Repulsion:
 Electrically charged group oriented on the
surface of emulsified globule produce
repulsive electrical forces between
approaching droplet due to electrical double
layers.
 This prevent the coalescence of globules.
 Ex. o/w emulsion stabilized by sodium soap.
(C17H35COO--Na+)
Theory of emulsification
Zeta potential:
 Zeta Potential is the electrical
potential that exists at the
"shear plane" of a particle,
which is small distance from its
surface.
 Zeta Potential is derived from
measuring the mobility
(velocity of particle/electric
field unit) distribution of a
dispersion of charged particles
as they are subjected to an
electric field.
 High zeta potential confer
Formulation of emulsion

A.Emulsifying agent:
B.Preservative:
C.Antioxidants:
D.Flavoring agent:
Emulsifying agent
Qualities required for good Emulsifying agent:
1. It should reduce surface tension below 10
dynes/cm.
2. It should be absorbed quickly on surface of
dispersed medium.
3. It should form coherent (non-adherent)
film.
4. It should be effective in low concentration.
5. It should increase viscosity and maintain
consistency.
Classification of emulsifying
agents
1. Natural:
a. Vegetable source: Gum acacia, tragacanth, agar,
starch, pectin, iris moss.
b. Animal source: wool fat, egg yolk, gelatin.
2. Semi synthetic: Methyl cellulose, Na CMC
3. Synthetic:
a. Anionic: Sodium Lauryl Sulphate
b. Cationic: Cetrimide, benzalkonium chloride.
c. Non-ionic: Glyceryl ester- glyceryl monoesters etc.
4. Inorganic: Milk of magnesia, Mg oxide, Mg trioxide etc.
5. Alcohols (polyoles): Carbowax, cholesterol and lecithin.
Natural emulsifying agents
a. Vegetable source:
i. Acacia:
 Emulsion is attractive, palatable and stable in ph 2-
5.
 Preferred in o/w type of emulsion.
 Low viscosity and form multimoleculer film around
globules
i. Tragacanth:
 Produce coarse, thick emulsion so rarely used.
 Improve viscosity so used in combination with
acacia.
i. Agar:
 It is not a good emulsifying agent.
Natural emulsifying agents
a. Vegetable source:
iv. Pectin:
 1% mucilage in water used as EA.
 It is incompatible with alkalis, strong alcohol, tannic
acid and salicylic acid.
iv. Starch:
 It is rarely used as it form coarse emulsion.
 It is used in preparation of enemas.
iv. Iris moss (chondrus):
 Thickening agent.
 Used in combination with acacia in cod-liver oil
emulsion.
 Concentration of 3% used as EA.
Natural emulsifying agents
b. Animal source:
i. Wool fat:
 Prepare external use emulsion, absorb 50% of
water.
 Produce o/w type of emulsion.
i. Egg yolk:
 Prepare internal use emulsion.
 Preservation in refrigerator.
 It used concentration of 12 to 15%
i. Gelatin:
 Used for emulsification of liquid paraffin emulsion.
 It produce white and agreeable taste emulsion.
 Concentration 1%, require preservation.
Semi-Synthetic Emulsifying
agent
a. Methyl cellulose:
 It is synthetic derivative of cellulose.
 It is used as suspending/thickening agent.
 Concentration of 2%.
 It form precipitate with electrolytes.

a. Sodium Carboxy Methyl Cellulose:


 It is used as emulsion stabilizer.
 It is used as suspending/thickening agent.
 Concentration of 0.5 to 1.0 %.
Synthetic emulsifying agents
a. Anionic:
 These are used in the preparation of external use
emulsion.
 Ex. Alkali soap, metallic soap, sulphated alcohol,
sulphonets.
 Sodium lauryl sulphate is sulphonated alcohol
produces o/w emulsion and form monomolecular film.
a. Cationic:
 Quaternary ammonium compound e.g. benzalkonium
chloride, cetrimide.
 Prepare external use preparation.
a. Non-ionic:
 Glyceryl mono stearate, sorbitan monopalmitate.
Inorganic emulsifying agent
a. Milk of magnesia:
 10 to 20%, prepare o/w coarse emulsion.
a. Magnesium oxide:
 5 to 10%, prepare o/w coarse emulsion.
a. Magnesium aluminium silicate:
 1% used to prepare o/w coarse emulsion.
a. Bentonite:
 5% is used to prepare o/w or w/o emulsion.
 When used in o/w emulsion oil is added to the
suspension of bentonite.
 for w/o emulsion oil is placed in bottle and suspension
of bentonite is added.
Alcohols / Polyoles
a. Carbowaxes(polyethylene glycol):
 Used to prepare cream and ointment.
 Molecular wt 200-700 viscous, light coloured,
hygroscopic liquid.
 Molecular wt 1000 and above are wax solid.
a. Cholesterol:
 Ex. Cetyl alcohol, stearyl alcohol, cholesterol.
 These are used to stabilize emulsion.
a. Lecithin:
 It form w/o emulsion.
 They are rarely used as they darken the preparation.
Selection of emulsifying agent
 HLB(hydrophilic lipophilic
balance) system:
1. It is derived by Graffin in
1949.
2. HLB system characterize
its relative polarity.
3. More the hydrophilic
interfacial barrier it
favour o/w emulsion and
while non polar barrier
favour w/o emulsion.
4. Oleic acid-1.8, Tween
80-15, SLS-40.
Preservatives
 Number of ingredients in emulsion support the
growth of microorganism which result into change in
colour, odour and taste of emulsion.
 Therefore there is need to include the preservative.
 Sources of contamination:
1. During the development or production.
2. Impure raw material.
3. Poor sanitation.
4. Improper ratio of o/w/gum.
5. pH change.
Preservatives
 Rules for prevention of contamination:
1. Use of uncontaminated raw material.
2. Meticulous house keeping.
3. Careful cleaning of equipment.
4. Maintenance of pH.
5. Maintain o/w/gum ratio.
 Qualities required in preservative:
1. Low toxicity.
2. Stable to heat and storage.
3. Chemical compatibility.
4. Reasonable cost.
5. Acceptable taste, odour and colour.
Preservatives
 Selection of preservative:
 Concentration of preservative required in an
emulsion depend on its ability to interact with
microorganism.
 The preservative selected on distribution
coefficient Ko/w .
 It should effective in both phase, soluble in both
phase.
Example:
 Esters of parahydroxy benzoic acid: benzoic
acid(0.1-2%), methyl paraben& propyl
paraben(0.1-2%), Chloroform (0.25%)
Antioxidants
 Many organic compound subjected to
autoxidation upon exposure to light and air
and result on decomposition.
 Emulsified lipid are particularly sensitive to

attach.
 Unsaturated oils become rancid on

autoxidation result in change in taste, odour


and appearance.
Example:
 Gallic acid, propyl gallate, ascorbic acid, butylated
hydroxytolune (BHT), butylated hydroxyanisol
Flavouring agent

Flavouring agent is incorporated in the


formulation to impart the taste to it.
Example:
 Vanillin – in liquid paraffin emulsion.
 Benzaldehyde – in cod-liver oil emulsion.
Methods of preparation

 Dry gum method.


 Wet gum method.
 Bottle method:
For volatile & non-viscous oils.
Other method
(homogenizer).
Methods of preparation
 Preparation of primary emulsion:
Sr. no Types of oils Example O/W/Gum

1 Fixed oil Caster oil 4:2:1

Almond oil

Arachis oil

Cod-liver oil

2 Volatile oil Turpentine oil

Peppermint oil 2:2:1

Cinnamon oil

3 Mineral oil Liquid paraffin 3:2:1


Example
Rx
Caster oil ----------- 8 ml
Water -------------- 30 ml
Prepare an emulsion
 Direction: One tablespoonful to be taken
before going to bed.
 Use: Laxative
Identification test for emulsion
Dilution test :
1. Emulsion will remain stable
by the addition of external
phase.
2. When water is added in to a
test tube containing
emulsion, if separation of oil
globules not occurs, the
emulsion is o/w type.
3. If the same is with oil, the
separation of oil globules
takes place leading to phase
Identification test for emulsion
Fluorescence test :
1. There are many oil
which glow in
presence of u. v. light.
2. Therefore, when
emulsion is observed
under microscope, if
globules shows
glowing then it is
concluded that the
preparation is o/w
type.
Identification test for emulsion
Conductivity test:
1. Water is good conductor of
electricity and oil is bad
conductor of electricity.
2. When electrodes dipped into
emulsion and connected to
battery,
3. light; if bulb glows, the
emulsion is o/w, as water is
external phase which
conduct the electricity.
Identification test for emulsion
Dye test:
1. The Water soluble
dye is mixed to an
emulsion and
observed under
microscope.
2. If the disperse
globules appear
colorless and the
background red.
3. This is o/w type of
Identification test for emulsion

Cobalt chloride paper test:


1. Anhydrous cobalt is blue in
color and hydrous cobalt is
red or pink in color.
2. When cobalt chloride paper
dip in emulsion, if the color
change occurs, from blue to
red or pink,
3. Preparation contains water
as an external phase so,
the emulsion is o/w type.
Stability of emulsion
 Garrett definition; A stable emulsion is one that
would “maintain the same number of sizes of
particle of the dispersion phase per unit volume
of weight of the continuous phase”.
 An emulsion is said to stable if it remains as
such after preparation to its shelf life.
 Following changes might be occurring:
1. Creaming.
2. Cracking.
3. Phase inversion.
Stability of emulsion
Creaming
 When large globules or aggregate of globules
rises to the top of an emulsion or fall to the
bottom and form concentrated thick layer.
 Temporary phase.
 Creaming should be avoided because it leads
to cracking.
 Stock law:
V = 2r2 (d1- d2) g

Creaming
 Factor affecting  Stock law:
creaming: V = 2r2 (d1- d2) g
1. Radius of

globules.
2. Density of
dispersion
medium/dispersin
g medium.
3. Viscosity.
4. Storage
condition.
Cracking
 Greater destruction to an emulsion than
creaming.
 It is the coalescence of the globules of
internal phase and separation of that phases
in to a distinct layer.
 This is irreversible, since the protective sheet
above the globules of the internal phase no
longer exist.
 Re-stabilization by shaking is normally
unsuccessful.
Cracking
 Reasons for cracking:
1. Addition of opposite
charged emulsifying
agent.
2. Decomposition/preci
pitation of
emulsifying agent.
3. Addition of common
solvent.
4. Microorganism.
5. Change in
temperature.
Phase inversion
 Phase inversion means change in the type of
emulsion i.e. o/w to w/o or vice versa
 Reasons for phase inversion.
1. Addition of electrolyte.
2. Changing phase volume ratio.
3. Temperature change.
4. Changing the emulsifying agent.
Evaluation of emulsion

1. Globular size analysis:


2. Centrifugation:
3. Viscosity:
4. Stress condition:
Aging and temperature
(Accelerated stability studies):
Any Question ???

Thank You