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Nano-Emulsion and Nano-Encapsulation of Fruit Flavor: Review

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International Conference on Food Science & Technology IOP Publishing
IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

Nano-Emulsion and Nano-Encapsulation of Fruit Flavor: Review

A Suyanto1,2, E Noor2, M S Rusli2, F Fahma2
1
Food Technology Department of University of Muhammadiyah Semarang
2
Department of Agroindustrial Technology, Bogor Agricultural University
Corresponding author: [email protected]

Abstract. Nano-emulsion and nano-encapsulation of fruit flavor aim to make flavor stabilization
which is generally labile in the form of liquid (emulsion) and powder (encapsulation) preparations.
Nanotechnology in food is a technology to reduce food particle size to 20-200 nm which is generally
followed by new properties both physical, chemical and sensory. In nano-emulsion products such as
transparent color and products stability are characterized by: absence of sedimentation (creaming),
unification of two particles (flocculation), unification of particles to enlarge (coalescent) and
exchange of internal and external phases (inversion). In nano-encapsulation products flavor stability is
maintained by reduced aroma volatility which is bound by the carrier matrix while controlling the
release of aroma. The method of forming nano-emulsion uses two approaches, namely high energy
such as high-pressure homogenization and ultra-sonication methods, and low energy such as
spontaneous emulsification. Making an emulsion is by mixing two different compounds of polarity
stabilized by the emulsifier. In the emulsion flavor system for making nano-encapsulation a
biopolymer is needed which acts as a core coating. The encapsulation was made by making an
emulsion first, then one of the drying techniques was carried out such as spray drying, drum drying
and freeze drying. This literature review describes nano-emulsion techniques and nano-encapsulation
of fruit flavor

Keywords: nano-emulsion, nano-encapsulation, fruit flavor, emulsifier, coating matrix

1. Introduction
1.1 Flavor Nano-Emulsion
Fruits have the preferred flavor, where different types of flavoring components for each different
type of fruit. ‘Kawista’ fruit, for example, which is classified as a tropical plant, identified using Gas
Chromatography-Mass Spectrometry (GC-MS) has 75 flavor components as volatile compounds, which
consist of esters, alcohols, aldehydes, ketones, lactones, heterocyclic aromatic, hydrocarbons, acetal, furan
and carboxylic acids [1]. Flavor compounds consist mostly of volatile components so that they are labile by
environmental conditions. Emulsion and encapsulation of flavor is one way to maintain flavor stability.
Nanotechnology can be applied in food processing technology in the form of nano-emulsion and
nano-encapsulation. The definition of nanotechnology in food processing is the manufacture of food
materials that are nano-scale, i.e. 20-200 nm. Nano-sized material designed in the order of the smallest atom
or molecule, has special properties compared to the origin of the material.
Nano-emulsion is often referred to as mini-emulsion, nano-emulsion, ultrafine emulsion, and
submicron emulsion. Nano-emulsion looks transparent and translucent which is seen with ordinary eyes and

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International Conference on Food Science & Technology IOP Publishing
IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

does not occur sedimentation (creaming) due to Brownian. One other hand, it is also resistant to flocculation
because efficiently of steric stability. The unique properties of the nano-emulsion can be categorized as nano-
emulsion having thermodynamic stability. Most nano-emulsions are stable by synthetic surfactants which
have long hydrophilic groups [2].
Emulsions consist of conventional emulsion (O/W and W/O), multiple emulsions (W/O/W),
multilayer emulsions (MO/W), solid lipid particles (SLP-O/W), and filled hydrogel particles (O/W/W).
Double emulsion of water in oil in water (W/O/W), where small water droplets contained in larger oil
droplets, will then be dispersed in a continuous water phase [3].

Figure 1. Emulsions type: Nano-emulsion (A), Lipid droplets (B), Filled Lipid droplets (C), solid lipid
nanoparticle (D), Multilayer emulsions (E), colloidomes (F)

Compounds in the form of nano-emulsion have stability to environmental influences. A stable

material is still within acceptable limits during the period of storage and use, which has the same
characteristics which are made. Physical instability of the material is characterized by the bleaching of colors
or the appearance of colors, odor arising, changes or separation of phases, rupture of the emulsion, deposition
of suspensions or caking, changes in consistency, crystal growth, gas formation and other physical changes.
Whereas, the stability of nano-emulsion is influenced by changes in physics and chemistry. Indicator that
becomes of the instability of nano-emulsions includes creaming, flocculation, coalescent and ostwald
ripening, and inversion.

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

Figure 2. Nanoemulsion destabilization [4]

Creaming is the emulsion phase separation based on the difference in density between the dispersed
phase and the continuous phase. Creaming is an undesirable process, but this condition can be dispersed
again with agitation. Creaming speed is influenced by several factors, namely based on the depositional
velocity theory stated by the Stokes law [5]. Flocculation is the incorporation of globules depending on the
electrostatic force (potential Zeta). This instability can still be improved by shuffling because the film
between the surfaces is still there [6].
Coalescent is the process by which the droplets of a phased approach and combine to form larger
particles and become a layer. This happens not only because of the surface free energy but also because not
all globules are coated by interface films [5]. This instability is more damage than creaming. Attempts to
stabilize this instability cannot be done by shuffling, usually additional emulsifiers and reprocessing are
needed [7].
Ostwald Ripening is the process by which small droplets turn large and form new droplets. This
phenomenon is related to systems that have varying droplet sizes. The phenomenon of coalescence and
Ostwald Ripening causes the separation of the system into three phases, namely the internal, external and
emulsifier phases. Inversion is an event where the external phase becomes an internal phase, and vice versa
[5].
There are two methods for forming nano-emulsions, namely the formation of using high energy and
low energy approach. High energy formation uses mechanical equipment capable of breaking oil and water
phases such as high-pressure homogenizers, micro-fluidizers, and sonication methods. The formation of low
energy nano-emulsion is produced as a result of phase transitions during the emulsification process where
there is a change in composition with constant temperature. The method often used is membrane
emulsification, spontaneous emulsification, emulsion inversion point, phase inversion point, solvent
displacement [8].
Emulsion formation can be done directly and indirectly, where the quality of the emulsion is better in
indirect emulsions [9]. The emulsion technique directly by mixing becomes one of all ingredient emulsions,
while the indirect emulsion is carried out in two stages, namely pre-emulsion and emulsion. The minimum
grain size that can be produced using each approach depends on several different factors. Reducing particle
size using a high-energy approach depends on the type and operating conditions of the homogenizer (eg
energy intensity, time and temperature), sample composition (eg oil type and concentration and emulsifier)
and physicochemical properties of component phases (eg interface voltage and viscosity).

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

Making fruit flavor nano-emulsion is expected to improve its color characteristics, particle size,
viscosity, pH, solubility and availability so that it will increase acceptance by consumers. The combination of
emulsifying materials and stabilizing fruit nano-emulsions will produce smaller emulsion grain sizes. Malto-
dextrin or inulin as a biopolymer is added as a thickener which aims to increase viscosity and slow down the
deposition process, so that the nano-emulsion produced will be more stable.

Table 1. Nano-emulsion flavor techniques that are bioactive components

Fruits (Flavor) Emulsion type Method Parameters References
and emulsifier
Orange (D- O/W. Sorbitan Emulsification two Droplet size, morphology [10]
limonene) trioleate and poly steps, (TEM) stability 14 weeks room
oxy-ethylene (20) homogenization temperature, electrophoretic
oleyl ether (HLB and sonication 20 (zeta potential),
1.8 and 15.0). co- kHz
surfactant
Ethylene glycol
Grape berries W/O continuous Vortex and Droplet size and stability 7 days [11]
phase lemongrass homogenizer ultra- at room temperature. Sensory
oil. Tween 80 thorax 10000 rpm analysis. Anti-microbial (disk).
continued dynamic Phenol total, anthocyanin,
high pressure (5000 antioxidant activity, degree
rpm) color
Medium-chain O/W. Gelatin. Spontaneous Droplet size (nano zetazier [12]
triglyceride Tween 80 homogenization ZS), turbidity, degree color,
(MCT) (magnetic stirrer stability, rheology
20oC and 60oC)
‘Temulawak’ O/W. Malto- Homogenization Curcumin Bio-availability, [13]
extract dextrin. Tween 24000 rpm (High- solubility, stability, index bias,
80 Speed pH, viscosity, droplet size
Homogenizer -
Virtis 23)
Zingerrol O/W. Tween 80 Low-temperature Droplet size, stability, bioactive [14]
extract homogenization compound, solubility, bio-
22000 rpm viability

1.2 Flavor Nano-encapsulation

Encapsulation technology is able to convert scents into stable compounds in the form of liquids, pastes,
powders, granules, capsules, microcapsules or nano-capsules. The form of encapsulation of the aroma will be
able to maintain, protect, reduce the power of volatility, stabilize, and control the release of aroma.
Variations in components that can be used as encapsulation matrices include starch, gelatin, or cyclo-dextrin
[15].
Encapsulation is a technique of trapping food components with a polymer coating, forming round nano-
capsules measuring between tens of nano to several microns. Encapsulation of flavor in nano-capsules can be
released at controlled speeds under certain conditions. Nano or micro-encapsulation techniques that are
widely used commercially are spray drying, air suspension coating, accreditation, spray cooling and spray
chilling, centrifugal extrusion, rotational suspension separation and inclusion complexion. Spray drying or
spray dryer is a widely used encapsulation technique [16].

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International Conference on Food Science & Technology IOP Publishing
IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

In general, flavor encapsulation techniques can be carried out chemically such as conservation, co-
crystallization, molecular complex, and interfacial polymerization; physically such as Spray drying, spray
chilling / cooling, extrusion, and fluidized beds [17, 18]. The advantages and disadvantages of each flavor
encapsulation technique are presented in Table 2.

Tabel 2. Advantages and disadvantages of flavor encapsulation method [19].

Encapsulation Advantages Disadvantages
method
Conservation Encapsulation efficiency of 40-90%, Expensive, complex mechanisms
Using organic solvents, (advance technology), sensitive to the
Applied to heat sensitive components environment, the presence of toxic
compounds such as glutaraldehyde

Co-Crystallization the method of entrapping (using Flavor sensitivity is quite high, rarely
sugar), the orange peel is quite good, used
but it is recommended to add
antioxidants

Spray drying Encapsulation efficiency of 10-90%, Not suitable for heat sensitive
Easy, low cost, high reproducibility, components, it is difficult to control
high productivity particle size

Spray Encapsulation efficiency 10-100%, It is not easy to control particle size,

cooling/spray The cost is cheaper than spray drying, Moderate yield on small scale
chilling suitable for heat sensitive components production

Freeze drying The quality of flavor is better than hot Expensive production costs, expensive
drying handling and storage in the long period

Fluidized bed Encapsulation efficiency 5-50%, Heat temperature will integrate the
coating Can control particle size, low cost, can flavor component
dry encapsulate multi-layer

Extrusion Encapsulation efficiency of 20-50%, Difficult in increasing scale

Can be used in aerobic and un-aerobic It is difficult for high viscosity
conditions polymers

Encapsulation makes flavor protected from adverse environmental influences such as damage due to
oxidation, hydrolysis, evaporation or heat degradation. Thus, flavor will have a longer shelf life and better
process stability. In addition, the release of material from the capsule can also be controlled so that its
effectiveness can be designed as desired. The challenge of the application of nano-encapsulation technology
lies in the selection of the nano-encapsulation technique and the appropriate encapsulating material (coating
wall) so that the capsule can function according to its purpose.
Some reasons for implementing nano-encapsulation in the food industry are: to reduce core reactivity with
environmental factors, reduce the transfer rate of core materials with the outside environment, to promote
easier handling, to control the release of core material, to cover the core taste, and melt core material when

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

must be used in small quantities [20]. In its simplest form, nano-capsules are small balls with uniform walls
around them. The material in nano-capsules is called the core, internal phase, or filler, while the wall is also
called shell, layer, material wall, or membrane. Nano-capsule can have several coating walls [21].
Nano-capsule coatings can use carbohydrate ingredients such as dextrin, sugar or starch. Other
ingredients can also come from proteins such as gelatin and soy protein. While one method commonly used
in industry is using a spray dryer. Coating materials commonly used for the spray drying process include
carbohydrates, Arabic gum, semi-synthesized cellulose derivatives and synthesis polymers [22). Each
coating material (carrier / coating) has advantages and disadvantages to the properties, price and
encapsulation efficiency. At present malto-dextrin, a modified starch derivative that can be dissolved, used
individually or in combination with other ingredients in the process of making food and medicines from plant
extracts, aromatic preservatives and vitamins [23].
Malto-dextrin has various aspects of function including enlargement and the properties of film formation, the
ability to bind taste and fat, and reduce the permeability of oxygen to the wall matrix. Some of the reasons
underlying maltodextrin for microencapsulation materials, according to Aakash [24] that maltodextrin can
reduce the reactivity of core material with an environment, controlled release which is suitable for core
material. Some microencapsulation studies using maltodextrin as coating wall material have been carried out
including the microencapsulation process of ginger oleoresin [25]. The highest microencapsulation efficiency
of ginger oleoresin with a ratio of 1: 16.7 (oleoresin: maltodextrin) with particle sizes of 1.05-12.90 µm.

Table 3. Nano-encapsulation of flavor and bioactive compounds

Material Encapsulation Wall matrix parameter References
method
Vanillin Spray drying Malto-dextrin, Yield, vanilla content, [26]
extract modified tapioca vanillin recovery, Aw,
Solubility, Morphology
(SEM)

Flavors (d- Spray drying Saccharomyces Component of flavor (GC- [27]

limonene, ethyl cereviceae MS), encapsulation
hexanoate, efficiency, particle size,
citral and ethyl moisture content,
propionate) morphology (SEM)

Red pepper coacervation Alginate yield, color, particle size, [28]

(ionic gelation substituted with water content, texture,
system) Tapioca is capcaicin content,
photooxidated encapsulation efficiency and
loading capacity
Temulawak Preparation by TPP and chitosan The yield, crystallinity [29]
extract ultra-sonication, (XRD), a complex group
spray drying (FTIR), size and
morphology (SEM)
PUFA (Sun Preparation by 2- Malto-dextrin Particle size, viscosity,%
flower) stage and agave inulin surface oil,
homogenization
and continued

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

Material Encapsulation Wall matrix parameter References

method
with spray drying

The application of the spray drying process to microencapsulation involves three basic steps [30],
namely preparation of dispersions or emulsions for processing, homogenization of dispersions, and
atomization of masses into the drying chamber. The first step is the formation of a good and stable emulsion
from the core material in a solution of the wall. The dispersion must be heated and homogenized, with or
without the addition of emulsifiers depending on the emulsifying properties of the coating material because
some have their own interfacial activity. Before the spray drying step, the emulsion formed must be stable for
a certain period of time, oil droplets must be rather small and the viscosity must be low enough to prevent the
entry of air in the particles [31].
In food products that do not heat stable such as flavor, the use of spray drying techniques needs to be
considered, considering the drying operating temperature can reach 180 oC. In flavor products the freeze-
drying technique in the encapsulation process is an alternative. The advantages of freeze-drying techniques
are that they can produce higher quality products because the products produced have a rigid structure due to
the sublimation process. Rigid structures make the product porous and do not contract at dry conditions.
Other advantages reduce the degradation of substances that are not heat resistant [32, 18].

2. Emulsifier
Emulsifiers and surfactants are two terms that have the same meaning. An emulsifier is an active ingredient
at the interface between two phases, a hydrophilic and hydrophobic phase. Emulsifiers have two groups in
one molecule, namely polar groups which remember polar compounds such as water and non-polar groups
which remember non-polar compounds such as oil. The unique nature of this emulsifier will be able to
reduce the surface tension of two compounds that cannot mix together to be able to mix.
The use of excessive emulsifiers will cause low solubility so that emulsifying crystals are formed.
The formation of these crystals will reduce their ability to form emulsions between fat and water. Imperfect
emulsion formation will cause fat to separate during the processing so that the resulting fat content decreases
[33].
The HLB (hydrophile-lipophile balance) value of an emulsifier is a number that shows a measure of
balance and strain of a hydrophilic group (like water or polar) and a lipophilic group (like oil or non-polar),
which is an emulsified two-phase system. HLB numbers are used to characterize emulsifiers. If the HLB
emulsifier number is high, the emulsifier will be more soluble in water, whereas if the HLB number is low,
the emulsifier will dissolve easily in oil.

Table 4. Use of HLB [34]

Nilai HLB Penggunaan

1-3 Anti foaming agent

3-6 W/O Emulgator
7-9 wetting agent
8-18 O/W Emulgator
13-15 Detergent
10-18 solubilizing agent

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The W/O/W emulsion consisting of W/O and O/W emulsions requires two emulsifiers to form two systems,
which must contain a low HLB (Hydrophile Lipophile Balance) value to stabilize the W/O emulsion and one
must contain an HLB value high to stabilize the O/W emulsion.

Table 5. HLB values of various types of emulsifiers

Kind of Emulsifier HLB Kind of Emulsifier HLB
Tween 20 16,7 Span 20 8,6
Tween 40 15,6 Span 60 4,7
Tween 80 15,0 Span 80 4,3
Tween 60 14,9 Arlacel 83 3,7
Tween 85 11,0 Gom 8,0
Tween 65 10,5 Trietanolamine 12,0

Tween 20 is a non-ionic hydrophilic surfactant which functions as an emulsifier, solvent, wetting

agent. Tween 20 is widely used as an emulsifier in the preparation of oil-in-water emulsions. Tween 20 has a
distinctive and warm odor, tastes rather bitter, yellow. Tween 20 is soluble in ethanol and water, and is
insoluble in mineral oil and vegetable oil. Tween 20 must be stored in a tightly closed container, protected
from light in a cool, dry place. Tween 80 emulsifier (polysorbate 80) in an oil in water (O/W) emulsion has
the chemical name poly-oxyethyene 20-sorbitan mono-oleate with formula formula C64H124O26. Tween 80
has a distinctive and warm odor, tastes rather bitter, yellow. Tween 80 is soluble in ethanol and water and is
insoluble in mineral oil and vegetable oil. Tween 80 is a group of nonionic surfactants wherein the
ingredients are hexanhydrous alcohols, alkaline oxide and fatty acid hydrophilic properties are given by the
oxyethylene free hydroxyl group [35].

Table 6. Dispersibility of emulsifiers in water based on HLB

Dispersibility Range of HLB
Not dispersed 1-4
A little dispersed 3-6
Dispersed like milk with gouging 6-8
Dispersed like milk with stable conditions 8-10
Dispersed combines a translucent solution to clear 10-13
Dispersed into a clear solution 13 +

Surfactants are divided into four groups i.e anionic surfactants, cationic surfactants, nonionic
surfactants, and amphoteric surfactants [33]. Anionic surfactant is a type of surfactant that has a negatively
charged molecule in the hydrophilic part due to the presence of a very large ionic group. Anionic surfactants
are surfactants whose alkyl parts are bound to an anion such as alkane sulfonate salt, olefin sulfonate salt, a
long chain fatty acid sulfonate salt.
Cationic surfactant is a type of positively charged surfactant in its hydrophilic group due to the
presence of ammonium salts, such as Quaternary Ammonium Salt (QUAT). Cationic surfactants are
surfactants in which the alkyl portion is bound to a cation, such as alkyl trimethyl ammonium, dialcyl-
dimethyl ammonium salt and dimethyl benzyl ammonium alkyl salt.
Nonionic surfactant is a type of surfactant that is not charged or does not occur molecular ionization
due to the presence of an ether or hydroxyl oxygen group. Nonionic surfactants are surfactants which are not
charged alcyl parts, such as fatty acid glycerin esters, fatty acid sorbitan esters, fatty acid sucrose esters,
polyethylene alkyl amines, glucamines, alkyl poly-glucosides, mono alkanol amines, dialkanol amines and
alkyl amine oxides.

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

Amphoteric surfactant is a type of surfactant that is positively and negatively charged on its
molecule, where the charge depends on pH, at a low pH it will be negatively charged and at a high pH
positively charged. For example surfactants that contain amino acids, betaine, phosphobetain.

3. Emulsion stabilizer
In the flavor emulsion system a biopolymer is needed as a core coating. The encapsulation process begins
with making the emulsion first, then drying it. In microencapsulation synthetic flavor to reduce flavor loss
and improve stability using biopolymers from native starch and starch modified succinylated and octenyl
succinylated. Corn and barley succinylated starch is more effective than native starch and oktenyl starch.
Succinylated starch shows the ability of flavor resistance compared to β-cyclodextrin which is widely used as
a Coating material in microencapsulation of essential oils or flavor Succinylate starch shows the ability of
flavor resistance compared to β-cyclodextrin which is widely used as a coating material in essential
microencapsulation of oil or flavor [36].

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

Wall Matrix of flavor

Polysaccharides Protein Lipid Polymer

Plant : starch, Plant : Zein, whey, Nan-oemulsion : 1. PLGA (poly lactide-co-

cellulose, gum soybean Triglyceride glycolide)
2. PVA (Poli vynil
Animal : chitosan Animal : gelatin, Nano-liposome:
alcohol)
Algae : alginate and casein/casienat Lisetin
3. PLA (Poli lactic acid)
derivate 4. PCL (poly ε-
Microbe : cyclo- caprolactone)
dextrin

Figure 3. Polymer coatings in nano-encapsulation [19]

Microencapsulation of cumin extract with modified starch as a coating is more tolerant of heat than
those using β-cyclodextrin [37]. During heating, β-cyclodectrin protects volatile compounds from
evaporation to 100oC while modified starch to 140oC. Protection of volatile compounds from heat by
maltodextrin depends on encapsulated material (160oC for limonene and 120oC for carvone).

Table 7. Types of coating matrices and their characteristics in flavor encapsulation [17]
Wall Matrix Characteristics Products
Carbohydrates Low cost and good retention Tuna oil; liquid tomato flavor
Malto-dextrin
Porous starches Effective absorption and sustained release, Coffee oil; limonene
simple production technology, and low cost
Hydrolyzed starches Excellent oxygen-barrier, low viscosity at Meat flavor; wasabi flavor
high solid level
Protein Excellent functional and nutraceutical β-Pinene; citronella
Milk proteins properties
Gelatin Early formation of surface crust, high Lime oil; lavender oil
emulsifying and stabilizing activities
Arabic gum Excellent emulsifying properties and Rosemary oil; mint oil
provides good volatile retention
Cyclo-dextrin Good resistance to oxidation, excellent Shiitake flavor; pine flavor
inclusion of volatiles
Liposomes Lipid bilayer that increases emulsifying and Resveratrol; sesame
emollient effects
Inulin Prebiotic effects, dietary fiber action, and Rosemary oil; olive oil
good solubility in water

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

Microencapsulation of the aroma components of d-limonene, ethyl hexanoate, octanal and 1-hexano used
native corn starch, acetylation modified corn starch and pre-gelatinization and maltodextrin. Malto-dextrin is
the most efficient coating material for flavor retention [38]. Gum Arabic is very effective as a coating
material because it can protect colloids well [39]. Gum Arabic can stabilize emulsions in a wide pH range.
Gum Arabic can be used in conjunction with other gum, carbohydrates and proteins.

4. Methode of Nano-emulsion and nano-encapsulation

4.1 Procedure of Fruit Flavor Nano-emulsion
Making nano-emulsion refer to Sanchez with modification [9]. The ingredients used are fruit flavor extract,
fruit flavor standard (Maltol, furaneol, benzyl acetate, hexyl acetat, Cis-3- Hexenol, trans-2-hexenal), citral,
lime, C8 aldehyde, acetyl pyridine), internal standard (D4 Pyrazin and 1,4-dichlorobenzene), nitrogen gas,
Tween 20, Pure water, whey protein concentrate, Malto-dextrin, β-cyclodextrin, Anhydrous Na2SO4,
Antimicrobial compounds, Acidity regulators.

4.1.1 Procedure of micro-emulsions

Micro-emulsions O/W are made by high-pressure homogenization techniques. Mixing of fruit flavor extract,
Tween 20, and pure water with 16000 rpm homogenizer (Ultra-Turrax T25, IKA, FR) for 3 minutes,
resulting in an emulsion of 30% w/w of oil in water.

4.1.2 Procedure of biopolymer solution

1. Prepare a solution of whey protein concentrate, β-cyclodextrin, Malto-dextrin and third mixture according
to the formula with pure water.
2. Add 0.02% sodium azide as an antimicrobial agent.
3. Stirring for 30 minutes using a magnetic stirrer at room temperature.
4. Standardize the solution at pH 6.0 using 0.1 M HCl then stored at room temperature.

4.1.3 Procedure of double W/O/W emulsions

W/O/W double emulsion is made gradually by adding O/W micro-emulsion into the aqueous biopolymer
phase with high-pressure homogenizer with different pressures of 35, 50 and 300 bar (high-pressure valve
homogenizer - 1001 L PANDA, Soavi NIRO, FR) at 16000 rpm for 5 minutes at 10oC, then emulsify again
with homogenizer 15000 rpm for 8 minutes at 10oC.

Flavor extract + Emulsifier + water

Homogenization I

Micro-emulsion Bio-polymer

Homogenization II

Nano-emulsion flavor extract

Figure 4. Procedure of Flavor nano-emulsion Fruit extract [9]

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

4.2 Procedure of Flavor Fruit Nano-encapsulation

To Manufacture of fruit flavor nano-encapsulation using spray drying. Encapsulation of double emulsions
into powders uses a spray drier (Model SP1500, Fanyuan Instrument Co., Shanghai, China) at a pressure of
2.5 bar, inlet temperature 140-150oC, outlet temperature 70-80oC, and average speed of 450 mL/h. Powder
stored in closed bottles was stored at 4oC for further analysis. The encapsulation method can be done by
freeze-drying technique. The mechanism of the encapsulation freeze-drying in flavor includes freezing the
emulsion, followed by drying by conditioning the ultra-high vacuum at 0.036 psi or about 0.0025 Bar so it
will sublimate to produce a solid product. Optimization of freeze-drying by setting the freezing temperature
(-10oC to -40oC) and processing time (18-30 hours).

Nano-emulsion flavor extract

Spray drying Freeze drying

Nanoparticles flavor extract

Figure 5. Procedure of flavor nano-encapsulation Fruit extract

4.3 Characteristics of nano-emulsion and nano-encapsulation

4.3.1 Droplet size, Poly-dispersity Index and stability
The size of the droplets from the nano-emulsion is determined by photon correlation spectroscopy. Droplet
measurements were carried out using the Zetasizer 1000 HS (Zetasizer Nano Zs, Malvern Instrument,
Malvern, UK). The data obtained include nano-emulsion droplet and poly-dispersity index (PdI) sizes. The
poly-dispersity index value (PdI) (0-1) provides information about the uniform size of an emulsion droplet.
The smaller the poly-dispersity index value shows the droplet size distribution is getting narrower, which
means the size of the droplet diameter is increasingly homogeneous. The stability of nano-emulsion size was
observed in three storage temperature conditions, then the size and dispersion of size measurements were
carried out using the PSA at the time of observation, which was day 0 to ... i.

4.3.2 Viscosity
The nature of viscosity and flow of liquid food products can be measured using an instrument called a
viscometer. The nano-emulsion viscosity was measured by Brookfield viscometer (LVDV Pro II, Brookfield
Engineering Laboratories, USA) with S34 spindles.

4.3.3 Color analysis

Nano-emulsions color evaluation using a spectrophotometer while observing nano-encapsulation surface
color using the image processing system, the results of the shooting are analyzed by software (Image j
1.47v).

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International Conference on Food Science & Technology IOP Publishing
IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

4.3.4 FTIR Analysis of Biopolymers

The structure of emulsifying biopolymers such as β cyclo-dextrin and inulin was tested by Fourier transform
infrared spectroscopy (FT-IR) using FT-IR spectrophotometer (Shimadzu, Japan) with reflection techniques.
The spectrum is observed in transmissions from 400 to 450 nm. Samples are mixed with KBr powder and
pressed into disk.

4.3.5 Scanning Electron Microscopy (SEM)

Nano-emulsion and nano-encapsulation flavor were placed on both sides of the plate then coated with a thin
layer of gold. Particle morphology was observed through emissions emitted by scanning electron microscope
(S-4160 Cold Field-Emission SEM, Hitachi, Tokyo, Japan) at 320 kV and photographed at a magnification
of 6000 times.

4.3.6 Analysis of Transmission Electron Microscope (TEM)

Nano-encapsulation morphology was visualized using transmission electron microscope (TEM). The sample
(50µl) was added to the 200 mesh copper-coated TEM holder sample (EM Sciences, Hatfield, PA, USA)
after being given a negative staining then observed with JEOL electron microscope JSM-1200EX II
(Peabody, MA, USA).

4.3.7 Measurement of encapsulation efficiency

Nano-encapsulation analysis of fruit flavor include total content and surface content.
Encapsulation efficiency is calculated using formula

Total extract of fruits flavor - extract free flavor in the supernatant

Encapsulation efficiency (%) = -------------------------------------------------------------------------------------
Total extract of fruits flavor

5. Conclusion
Nano-emulsion is a nano-sized disperse (<100nm) with two different of polarity stabilized by the emulsifier.
Fruit flavors which are dominated by volatile compounds are labile so they need to be stabilized in the
emulsion system. The characteristics of nano-emulsion are very good for maintaining physical and chemical
stability such as being transparent and preventing the separation of the emulsion phase. The formulation of
the dispersing phase composition, dispersed phase, type and quantity of emulsifiers, homogenization process
conditions greatly influenced the physical and chemical characteristics of fruit nano-emulsion flavor.
Nano-encapsulation is the binding of core compounds by coating both bio and synthetic polymer, from the
emulsion system formed and then dried to obtain nano-sized powder (<200nm). The formulation of the
dispersing phase composition, dispersed phase, type and number of emulsifiers, polymer group coating
material, homogenization process conditions, and type of drying technique greatly influenced the physical
and chemical characteristics of the nano-encapsulation of fruit flavor.

Acknowledgment
BUDI-DN Scholarship cooperation between the Ministries of Research, Technology and Higher Education
with the Ministry of finance. Also, Postgraduate Grant Program the Ministry of Research, Technology and
Higher Education of the Indonesian Government in 2018.

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IOP Conf. Series: Earth and Environmental Science 292 (2019) 012025 doi:10.1088/1755-1315/292/1/012025

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