FORMATION OF VITAMIN E

ENRICHED NANO EMULSION

AND ITS STABILITY
CHARACTERISTICS

Presented by : Ayush Kumar Barik Under Supervision Of

Rohan Bhoi Mr. Veda Prakash
Prateek Minz Assistant Professor
Manasi Lata Behera Department of Chemical Engineering
V. S. S. U. T, BURLA
 Nano emulsion
 Nano emulsions are oil-in-water (O/W), water-in-oil (W/O) dispersion of two immiscible
liquids stabilized using an appropriate surfactant. The mean droplet diameter attained is
usually less than 500 nm

 Their size varies from 10 to 1,000 nm.

  It is a thermodynamically unstable system, which can be stabilized by the presence of an

emulsifying agent (emulgent or emulsifier). The dispersed phase is also known as internal
phase or the discontinuous phase while the outer phase is called dispersion medium,
external phase or continuous phase. The emulsifying agent is also known as intermediate
or interphase.
Methods for preparation of nano emulsion
It broadly classified into two primary categories:
High energy method
Low energy method

High energy method:-

High energy methods such as high pressure homogenization (HPH) and ultrasonication consume
significant energy to make small droplets.
The high-energy emulsification method includes high-energy stirring, ultrasonic emulsification, high-
pressure homogenization, micro fluidization, and membrane emulsification.

Low energy method:-

Low energy methods exploit specific system properties to make small droplets without consuming
significant energy . Phase inversion temperature and emulsion inversion point.
The low-energy emulsification method includes phase inversion temperature, emulsion inversion point,
and spontaneous emulsification.
 THEORY OF NANO EMULSIONS
 Oil-in-water emulsions and nano emulsions are commonly used in the food, cosmetics, healthcare,
supplement and pharmaceutical industries to encapsulate, protect, and release non-polar compounds.
These non-polar compounds may be nutrients, nutraceuticals, vitamins, antioxidants, antimicrobials,
colors, flavors, or drugs. The non-polar compounds may form the entirety of the disperse phase
within an emulsion (e.g., fish, flaxseed, essential, or flavor oils) or they maybe dissolved in carrier
oils (e.g., carotenoids or vitamins dissolved in corn oil). The physicochemical properties, sensory
attributes, and gastrointestinal fate of oil-in-water emulsions depend on their microstructure and
composition.

 Consequently, emulsions with different functional attributes can be fabricated by carefully

controlling their microstructure and composition. This is usually achieved by selecting specific
components to formulate the emulsion (such as surfactants, co-surfactants, oils. An understanding of
the physics of nano emulsion formation is critical for the control of nano emulsion droplet size.
 Nano emulsions are typically prepared in a two-step process where a macroemulsion is first prepared, and is
then converted to a nano emulsion in a second step. In this section, we describe various methods developed
over the past decade or so to prepare nano emulsions, and indicate the progress made on the prediction and
control of nano emulsion droplet size.
TYPES OF EMULSIONS
 O/W and W/O macroemulsions: These usually have a size range of 0.1–5 μm with an average of 1–2 μm.
 Nano emulsions: these usually have a size range of 20–100 nm. Similar to macroemulsions, they are only
kinetically stable.
 Micellar emulsions or microemulsions: these usually have the size range of 5–50 nm. They are
thermodynamically stable.
 Double and multiple emulsions: these are emulsions-of-emulsions, W/O/W, and O/W/O systems.
 Mixed emulsions: these are systems consisting of two different disperse droplets that do not mix in a
continuous medium.
BREAKDOWN PROCESSES IN EMULSION

The various breakdown processes are illustrated in figure. the physical

phenomena involved in each breakdown process are not simple, and it
requires analysis of the various surface forces involved. model
emulsions, with monodisperse droplets, cannot be easily produced, and
hence, any theoretical treatment must take into account the effect of
droplet size distribution. in addition, measurements of surfactant and
polymer adsorption in an emulsion are not easy and one has to extract
such information from measurement at a planer interface.
In the following sections, a summary of each of the above-mentioned
breakdown processes and details of each process and methods of its
prevention are given.

Creaming and Sedimentation : This process results from external

forces usually gravitational or centrifugal. When such forces exceed the
thermal motion of the droplets, a concentration gradient builds up in the
system with the larger droplets moving faster to the top (if their density
is lower than that of the medium) or to the bottom (if their density is
larger than that of the medium) of the container.
 Flocculation : This process refers to aggregation of the droplets
(without any change in primary droplet size) into larger units.
Flocculation occurs when there is not sufficient repulsion to keep the
droplets apart to distances where the van der Waals attraction is weak.
 Ostwald Ripening : This results from the finite solubility of the
liquid phases. Liquids that are referred to as being immiscible often
have mutual solubilities that are not negligible. With emulsions,
which are usually polydisperse, the smaller droplets will have larger
solubility when compared with the larger ones (due to curvature
effects).
 Coalescence : This refers to the process of thinning and disruption of
the liquid film between the droplets with the result of fusion of two or
more droplets into larger ones. The limiting case for coalescence is
the complete separation of the emulsion into two distinct liquid
phases.
 Phase Inversion : This refers to the process whereby there will be an
exchange between the disperse phase and the medium. For example,
an Oil in Water emulsion may with time or change of conditions
invert to a Water in Oil emulsion.
EXPERIMENT

AIM – Formation Of Vitamin E Enriched Nano Emulsion

CHEMICALS REQUIRED
Distilled water
Tween - 80(surfactant)
Coconut Oil
Vitamin E
EQUIPMENT REQUIRED
Magnetic type stirrer
Spatula
Beaker
Dynamic Light Scattering
Electron microscopy
 PREPARATION METHOD

 5 gm Tween 80(surfactant) was dissolved in 2 gm Vitamin E and 3 gm coconut oil at room

temperature in a beaker. The 90 gm distilled water was added slowly and the mixture was shaken
with a magnetic type stirrer for 20 minutes to get a homogeneous solution.

 The stirring time was fixed for 20 minutes in all cases. The only change took place is the varying
rpm of the magnetic type stirrer. Stirring generates intensive and disruptive forces in order to
minimize Nano emulsion droplets.

 Nano emulsions compositions prepared in this study are listed in Table 1. The water phase was
added into the oil phase (Vitamin E and surfactants) while stirring at 500 rpm and 750 rpm, at
temperature 33°C while stirring.
Composition of formulation characterized as nano
emulsions

Coconut Tween Vitamin Distilled Temperature Rotations per

oil (in 80 (in E(in gms) water (in (in °C) minute(rpm)
gms) gms) gms)

3.00 5.00 2.00 90.00 33 500

3.00 5.00 2.00 90.00 33 750

GRAPHICAL RESULT OF NANO EMULSION FROM DYNAMIC LIGHT
SCATTERING (DLS)
PROPERTIES

Nano emulsions have unique properties such as small droplet size, exceptional stability, transparent
appearance and tunable rheology. These properties make nano emulsions an attractive candidate for
applications in the food, cosmetic, pharma-ceutical industries and in drug delivery applications.
Furthermore, they can serve as the building blocks for designer advanced materials with unique
properties.

A stable nano emulsion is characterized by the absence of the internal phase, absence of creaming,
absence of deterioration by microorganisms, and maintenance of elegance in respect of appearance,
color, odor and consistency.
 EVALUATION AND PARAMETER OF NANO EMULSION

PH

 Monitoring the pH value is important for determining the emulsions' stability because pH changes indicate the
occurrence of chemical reactions that can compromise the quality of the final product. Emulsions produced with
vegetable oils may experience a decrease in pH due to the hydrolysis of fatty acid esters into free fatty acid
degradation products

  The high temperature might have destabilized the nano emulsion by hydrolysis, but it did not affect the overall
quality of the nano emulsions because the pH values remained around pH 6.0, which is an acceptable, non-skin
irritating pH value.

Physical-chemical analyses

 All nano emulsions were characterized by measuring their physicochemical properties; pH and conductivity.
Conductivity is the ability to conduct electrical current between two points. Electrical conductivity of the nano
emulsions was determined to check the stability and nature of the formulation. Conductivity measurement provides
information about continuous phase of nano emulsions (oil or water continuous) and phase inversion phenomenon.
Higher value of Nano emulsion conductivity points out more water content which provides more spaces for ions
movements. If the conductivity stays stable after storage at room temperature, it can be assigned as a sign of stability
without phase inversion.
 Droplet size analysis

 The dimensions of the droplets in an oil-in-water emulsion also have a pronounced impact on its
properties. The optical properties of emulsions are largely determined by the light scattering efficiency
of the droplets, which depends on their size relative to the wavelength of light. When the droplets are
much smaller than the wavelength of light (d < 50 nm), they only scatter light waves weakly and
therefore appear transparent or only slightly turbid. When the droplets have dimensions similar to the
wavelength of light (d = 100 nm to 10 nm), then they scatter light waves strongly and the emulsion
appears highly turbid or opaque. When the droplets are much larger than the wavelength of light (d >
50 nm), then they again scatter light weakly and the system appears less turbid or opaque. The droplet
size also plays a critical role in determining the long-term stability of emulsions.
 Disperse Phase Composition

 Oil-in-water emulsions can be prepared using a variety of different oils (which may be pure substances
or mixtures), which provides some flexibility over the disperse phase composition. Oils with different
densities, viscosities, interfacial tensions, polarities, solvent properties, and nutritional attributes can be

utilized depending on the application .

 Storage Stability of Nano emulsions

 One of the main aspects of preparation of essential oil nano emulsions is their stability against Ostwald ripening.
Ostwald ripening is the growth of large oil droplets at the expense of smaller oil droplets due to diffusion of oil
molecules through the intervening aqueous phase. For using nano emulsions as antimicrobial or antibacterial
agents in delivery systems, having good long-term stability is essential. The particle size changes in thyme oil
emulsions were evaluated by DLS method after storage at room temperature (25°C) for 60 days. When particle
size distributions of emulsions prepared with Tween 80 blend were compared before and after 2 months storage at
room temperature several trends were observed. The growth of particle size was observed for all the emulsions.
 Droplet Charge and Other Interfacial Properties

 The thin layer of emulsifier molecules that coats the oil droplets in an oil-in-water emulsion also has a pronounced
influence on its functional attributes. The charge, thickness, packing, and chemical reactivity of the interfacial
layer can be controlled by selecting appropriate emulsifiers and solution conditions (such as pH, ionic strength,
and temperature). Interfacial properties have a major impact on the physical stability of emulsions. For example,
the strength of the electrostatic repulsion between oil droplets tends to increase as their electrical potential
increases, whereas the strength of the steric repulsion increases as the thickness of the interfacial layer increases.
 Advantages of Nano emulsion
a.It may be used as substitute for liposomes and vesicles.

b.It improves the bioavailability of drug.

c.It is non-toxic and non-irritant in nature.

d.It has improved physical stability.

e.Nano emulsions have small-sized droplets having greater surface area providing greater
absorption.

f.It can be formulated in variety of formulations such as foams, creams, liquids, and sprays.

g.It provides better uptake of oil-soluble supplements in cell culture technology.

h.It helps to solubilize lipophilic drug.

i.Helpful in taste masking.

j.Less amount of energy is required.

 Disadvantages of Nano emulsion

a. Use of a large concentration of surfactant and co surfactant necessary for stabilizing the
nanodrops.

b. Limited solubilizing capacity for high melting substances.

c. The surfactant must be non-toxic for using pharmaceutical application.

d. Nano emulsion stability is influenced by environmental parameters such as temperature

and PH. these parameters change upon nano emulsion delivery to patients.
 Application
 Nano emulsion are finding application in diverse area such as drug
delivery, food, cosmetics, pharmaceutical and material synthesis.

 In drug delivery: where o/w nano emulsions have been used to deliver
hydrophobic drugs.

 In food industry: where flavored nano emulsions with improved

curcumin and digestibility have been prepared.

 In cosmetic industry: where nano emulsion has been tested for skin
hydration and ease of application.

 In pharmaceuticals: it may also protect the drug which are susceptible

to hydrolysis and oxidation.

 Nano emulsion have also been used as building blocks for complex
matrix synthesis such as compartmentalization nanoparticles and
encapsulated oil drop lets.
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