Desai, Park - 2005 - Recent Developments in Microencapsulation of Food Ingredients PDF
Desai, Park - 2005 - Recent Developments in Microencapsulation of Food Ingredients PDF
Desai, Park - 2005 - Recent Developments in Microencapsulation of Food Ingredients PDF
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Drying Technology: An
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Recent Developments in
Microencapsulation of Food
Ingredients
Kashappa Goud H. Desai
a
& Hyun Jin Park
a
a
Graduate School of Biotechnology, Korea
University, Sungbuk-ku, Seoul, South Korea
Available online: 06 Feb 2007
To cite this article: Kashappa Goud H. Desai & Hyun Jin Park (2005): Recent
Developments in Microencapsulation of Food Ingredients, Drying Technology: An
International Journal, 23:7, 1361-1394
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Recent Developments in Microencapsulation of
Food Ingredients
Kashappa Goud H. Desai and Hyun Jin Park*
Graduate School of Biotechnology, Korea University, Sungbuk-ku,
Seoul, South Korea
Abstract: Microencapsulation involves the incorporation of food ingredients,
enzymes, cells, or other materials in small capsules. Microcapsules offer food pro-
cessors a means with which to protect sensitive food components, ensure against
nutritional loss, utilize otherwise sensitive ingredients, incorporate unusual or
time-release mechanisms into the formulation, mask or preserve flavors and aro-
mas, and transform liquids into easily handled solid ingredients. Various techni-
ques are employed to form microcapsules, including spray drying, spray chilling
or spray cooling, extrusion coating, fluidized-bed coating, liposome entrapment,
coacervation, inclusion complexation, centrifugal extrusion, and rotational
suspension separation. Recent developments in each of these techniques are
discussed in this review. Controlled release of food ingredients at the right place
and the right time is a key functionality that can be provided by microencapsulation.
A timely and targeted release improves the effectiveness of food additives, broadens
the application range of food ingredients, and ensures optimal dosage, thereby
improving the cost effectiveness for the food manufacturer. Reactive, sensitive, or
volatile additives (vitamins, cultures, flavors, etc.) can be turned into stable ingre-
dients through microencapsulation. With carefully fine-tuned controlled-release
properties, microencapsulation is no longer just an added-value technique, but the
source of totally new ingredients with matchless properties.
Keywords: Microencapsulation; Food ingredients; Controlled release; Spray
drying; Microcapsules
INTRODUCTION
Microencapsulation is defined as a technology of packaging solids,
liquids, or gaseous materials in miniature, sealed capsules that can release
C, as well
as hard mono- and diacylglycerols with melting points of 4565
C.
[31]
In spray-chilling, the coating material is typically a fractionated or hydro-
genated vegetable oil with a melting point in the range of 3242
C.
[61]
In
spray-chilling, there is no mass transfer (i.e., evaporation from the ato-
mized droplets); therefore these solidify into almost perfect spheres to
give free-flowing powders. Atomization gives an enormous surface area
and an immediate as well as intimate mixing of these droplets with the
cooling medium. Microcapsules prepared by spray-chilling and spray-
cooling are insoluble in water due to the lipid coating. Consequently,
these techniques tend to be utilized for encapsulating water-soluble core
materials such as minerals, water-soluble vitamins, enzymes, acidulants,
and some flavors.
[62]
Fluidized-Bed Coating
Originally developed as a pharmaceutical technique, fluidized-bed coat-
ing is now increasingly being applied in the food industry to fine-tune
the effect of functional ingredients and additives. The main benefits of
such miniature packages, called microcapsules, include increased shelf
life, taste masking, ease of handling, controlled release, and improved
aesthetics, taste, and color. Fluidized-bed coating increasingly supplies
1372 Desai and Park
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the food industry with a wide variety of encapsulated versions of food
ingredients and additives.
[63]
Compared to pharmaceutical fluidized-bed
coating, food industry fluidized-bed coating is more obliged to cut
production costs and, therefore, should adopt a somewhat different
approach to this rather expensive technology. Solid particles are sus-
pended in a temperature and humidity-controlled chamber of high-
velocity air where the coating material is atomized.
[64,65]
Typical food
processing applications of fluidization include freezing and cooling, dry-
ing, puffing, freeze-drying, spray-drying, agglomeration and granulation,
classification, and blanching and cooking.
[66]
Great variations in avail-
able wall materials exist. Cellulose derivatives, dextrins, emulsifiers,
lipids, protein derivatives, and starch derivatives are examples of typical
coating systems, and they may be used in a molten state or dissolved in an
evaporable solvent. This technique is applicable for hot-melt coatings
such as hydrogenated vegetable oil, stearines, fatty acids, emulsifiers,
and waxes, or solvent-based coatings such as starches, gums, maltodex-
trins. For hot melts, cool air is used to harden the carrier, whereas for
solvent-based coatings, hot air is used to evaporate the solvent. Hot-melt
ingredients release their contents by increasing the temperature or physi-
cal breakage, whereas water-soluble coatings release their contents when
water is added. Fluidized-bed encapsulation can be used to isolate iron
from ascorbic acid in multivitamins and in small tablets such as childrens
vitamins. Many fortified foods, nutritional mixes, and dry mixes, contain
fluidized-bedencapsulated ingredients. Citric acid, lactic acid, sorbic
acid, vitamin C, sodium bicarbonate in baked goods, and salt added to
pretzels and meats are all encapsulated. Nowadays, the applicability
and the utility of fluidized-bed coating and other microencapsulation
techniques in the food industry is well recognized, as presented in several
reviews.
[6670]
There are, however, important factors to be considered in
fluidized-bed coating of food ingredients and additives.
Fluidized-bed coating was first developed by D.E. Wurster in the
1950s; hence, the term Wurster process.
[70]
Today, the fluidized-bed
coating method is being modified by changing the position of the nozzle
to be used for coating the solid particles. The different fluidized-bed coat-
ing methods are: (1) top-spray, (2) bottom-spray, and (3) tangential-
spray. The conventional top-spray method is shown in Fig. 4. The air
is passed through a bed of core particles to suspend them in air and coat-
ing solution is sprayed countercurrently onto the randomly fluidized
particles. The coated particles travel through the coating zone into the
expansion chamber, and then they fall back into the product container
and continue cycling throughout the process.
[71]
The top-spray system
has successfully been used to coat materials as small as 100 mm.
[71]
How-
ever, Thiel and Nguyen demonstrated the possibility of encapsulating
very fine particles (25 mm) by adsorbing them on a coarser carrier, which
is encapsulated by means of conventional fluidized-bed equipment.
[72]
In
Microencapsulation of Food Ingredients 1373
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the top-spray configuration, controlling the distance the droplets travel
before contacting the substrate is impossible, and coating imperfections
can occur due to premature droplet evaporation.
The bottom-spray method known as the Wurster system (Fig. 5) is
widely used for coating particles as small as 100 mm. In this method,
the particles are recycled through the coating zone at a faster rate and
the fluidization pattern is much more controlled than the top-spray
method.
[73]
The typical advantage of this method is that, the path of
the droplets concurrently toward the core particles is extremely short,
Figure 4. Top-spray fluidized-bed coating.
Figure 5. Bottom-spray fluidized-bed coating.
1374 Desai and Park
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so that premature droplet evaporation is almost absent. In addition,
coating solution can spread out at the lowest viscosity, producing a very
dense film with a superior physical strength. In contrary, Wesdyk et al.
reported that particles coated in the bottom spray mode did not display
a uniform film thickness with respect to particle size; larger beads dis-
played thicker films compared with smaller beads. The film thickness
variation could be explained by differences in fluidization patterns. This
phenomenon did not occur in other configurations.
[74]
Recently, a fascinating advancement in fluidized-bed coating tech-
nique was reported by Matsuda et al. for the fluidization and coating
of very fine particles.
[75]
In conventional fluidized-bed coating, whether
it is top-spray, Wurster, or rotational, the basic concept of fluidization
relies on the compensation of the gravitational force experienced by the
particles by an upward moving air flow, which ensures complete fluidi-
zation of the particles. Typical fluidized-bed apparatus can efficiently
process particles from 100 mm to a few millimeters. However, for very
small particles, other forces, such as electrostatic forces, start to play
a major role in the movement of the particles in the fluidization cham-
ber and prevent adequate fluidization. Colloidal particles have been
used with some success to reduce electrostatic force, but are not much
help in the fluidization of very small (submicron) particles in a conven-
tional fluidized-bed apparatus. In this innovative process (Fig. 6), how-
ever, the gravitational force is multiplied through the use of a rotating
perforated drum that contains the particle. The air flow is then applied
tangentially to the rotation of the drum as compensation for the gravi-
tational force, now a multiple (up to 37 g) of the normal gravitational
force.
The conventional top-spray method remains unique and widely used
technique in food industry. This is due to its high versatility, relatively high
batch size, and relative simplicity.
[75]
Recently, continuous fluidized-bed
Figure 6. Tangential-spray fluidized-bed coating.
Microencapsulation of Food Ingredients 1375
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coaters have been developed.
[76]
With such a continuous fluidized-bed
coating process, manufacturers can adapt the system to their own specific
requirements while maintaining the flexibility needed for a large material
throughput and wide product ranges, and while providing the coating
quality demanded in the food industry. The efficiency of fluidized-bed
techniques is governed by process variables, ambient variables, and ther-
modynamic factors (Table 3). Appropriate modification or combinations
of these variables will yield the desired results.
The use of melted fats, waxes, or emulsifiers as shell materials is a
relatively new but very promising and interesting concept. From an
industrial point of view, the inherent advantage of hot-melt fluidized-
bed coating lies in the fact that the coating formulation is concentrated
(no solvent, as in aqueous-based coating formulation), which means
dramatically shorter processing times. The energy input is also much
lower than with aqueous-based formulation since no evaporation needs
to be done. Very few reports have been published on hot-melt coating
by fluidized beds since Jozwiakowsksi et al. described the coating of
sucrose particles with partially hydrogenated cottonseed oil and analyzed
the optimal processing parameters by modified central composite
design.
[77]
A number of patent applications, very similar in processing
designs, have been published using fats and emulsifiers of various melting
points and have developed an innovative fluidized-bed process for coat-
ing particles with fats and waxes using supercritical carbon dioxide as the
solvent for the coating formulation.
[7880]
Here, again, minimal energy
input is needed to evaporate the solvent and the process might lead to
lower cost-in-use encapsulated ingredients.
Table 3. Different variables influencing fluidized-bed operation
No Variables
1 Process variables
1. Inlet air temperature
2. Inlet air velocity
3. Spray rate
4. Solution temperature
5. Solution dry matter content
6. Atomization pressure
2 Ambient variables
1. Ambient air temperature
2. Ambient air relative humidity
3 Thermodynamic
1. Outlet air temperature
2. Outlet air relative humidity
1376 Desai and Park
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APPLICATION OF FLUIDIZED-BED TECHNIQUE
IN FOOD INDUSTRY
This technique is used to encapsulate nutritional substances such as
vitamin C, B vitamins, ferrous sulfate, ferrous fumarate, sodium ascor-
bate, potassium chloride, and a variety of vitamin=mineral premixes.
These encapsulated products are used as nutritional supplements.
[81]
In
the case of bakery products, it is also used to encapsulate the leavening
system ingredients, as well as vitamin C, acetic acid, lactic acid, potass-
ium sorbate, sorbic acid, calcium propionate, and salt.
[81,82]
In the meat
industry, several food acids have been fluid-bed encapsulated to develop
color and flavor systems. They are also used to achieve a reproducible pH
in cured meat products and to shorten their processing time. Fluid-bed
encapsulated salt is used in meats to prevent development of rancidity,
as well as premature set due to myofibrilar binding.
[81]
Extrusion
Encapsulation of food ingredients by extrusion is a relatively new process
compared to spray-drying. Extrusion used in this context is not same as
extrusion used for cooking and texturizing of cereal-based products. Actu-
ally, extrusion, as applied to flavor encapsulation, is a relatively low-
temperature entrapping method, which involves forcing a core material in
a moltencarbohydrate mass through a series of dies into a bathof dehydrat-
ing liquid. The pressure and temperature employed are typically <100 psi
and seldom 115
C.
[23]
The coating material hardens on contacting the
liquids, forming an encapsulating matrix to entrap the core material. Then
the extruded filaments are separated from the liquid bath, dried, and
sized.
[12]
The carrier used may be composed of more than one ingredient,
such as sucrose, maltodextrin, glucose syrup, glycerine, and glucose.
[70]
Schultz et al. were pioneers in the extrusion=encapsulation pro-
cesses.
[83]
They emulsified orange peel oil in a molten dextrose mass, poured
it on stainless steel sheets, and let it cool. The pulverized product exhibited
good stability and flavor retention over a 6-month period. Combining the
basic formulation of Schultz et al. with extrusion, Swisher created a novel
encapsulating processes that is similar to the one currently used today in
the flavor industry.
[84]
The primary benefit claimed was the maintenance
of fresh flavor in encapsulated citrus oils, which otherwise would readily
oxidize and yield objectionable off-flavors during storage. He conducted
an accelerated shelf life test on encapsulated orange peel oil that contained
an antioxidant and found that its shelf life was about one year. Figure 7
shows the key steps for the flavor encapsulation by extrusion.
The advantage of this method is that the material is completely sur-
rounded by the wall material (true encapsulation), and any residual oil or
Microencapsulation of Food Ingredients 1377
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core material is removed from the surface in an alcohol bath.
[14,51,71,81]
This provides an excellent stability against oxidation and therefore pro-
longs the shelf life. The product can be kept for 12 years without any
substantial quality degradation.
[71,81]
This technique can be classified as
a glass encapsulation system or a controlled-release system, depending
on the polymeric materials used. The polymer matrices and the plastici-
zers used can be modified to produce the capsules for controlled release
in food application.
[85]
However, microcapsules produced from this
method are commonly designed to be soluble in water by the use of
high-molecular-weight hydrophilic polymer. Thus, this encapsulation
technique is considered unsuitable for subsequent extrusion processing
because the water in the extruder melt can dissolve the capsules.
[86]
Centrifugal Extrusion
Centrifugal extrusion is another encapsulation technique that has been
investigated and used by some manufacturers. A number of food-approved
Figure 7. Flow diagram of encapsulation of food flavors by extrusion method.
1378 Desai and Park
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coating systems have been formulated to encapsulate products such as
flavorings, seasonings, and vitamins. These wall materials include gela-
tin, sodium alginate, carrageenan, starches, cellulose derivatives, gum
acacia, fats=fatty acids, waxes, and polyethylene glycol. Centrifugal
extrusion is a liquid coextrusion process utilizing nozzles consisting of
concentric orifice located on the outer circumference of a rotating cyl-
inder (i.e., head). The encapsulating cylinder or head consists of a con-
centric feed tube through which coating and core materials are pumped
separately to the many nozzles mounted on the outer surface of the
device. While the core material passes through the center tube, coating
material flows through the outer tube. The entire device is attached to a
rotating shaft such that the head rotates around its vertical axis. As the
head rotates, the core and coating materials are co-extruded through
the concentric orifices of the nozzles as a fluid rod of the core sheathed
in coating material. Centrifugal force impels the rod outward, causing it
to break into tiny particles. By the action of surface tension, the coating
material envelops the core material, thus accomplishing encapsulation.
The microcapsules are collected on a moving bed of fine-grained starch,
which cushions their impact and absorbs unwanted coating moisture.
Particles produced by this method have diameter ranging from 150 to
2000 mm.
[87]
Lyophilization
Lyophilization, or freeze-drying, is a process used for the dehydration of
almost all heat-sensitive materials and aromas. It has been used to encap-
sulate water-soluble essences and natural aromas as well as drugs. Except
for the long dehydration period required (commonly 20 h), freeze-drying
is a simple technique, which is particularly suitable for the encapsulation
of aromatic materials. The retention of volatile compounds during the
lyophilization is dependent upon the chemical nature of the system.
[88]
Coacervation
Coacervation involves the separation of a liquid phase of coating
material from a polymeric solution followed by the coating of that phase
as a uniform layer around suspended core particles. The coating is then
solidified. In general, the batch-type coacervation processes consist of
three steps and are carried out under continuous agitation.
1. Formation of a three-immiscible chemical phase
2. Deposition of the coating
3. Solidification of the coating
Microencapsulation of Food Ingredients 1379
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In the first step, a three-phase system consisting of a liquid manufac-
turing vehicle phase, a core material phase, and a coating material phase
is formed by either a direct addition or in situ separation technique. In
the direct addition approach, the coating-insoluble waxes, immiscible
solutions, and insoluble liquid polymers are added directly to the
liquid-manufacturing vehicle, provided that it is immiscible with the
other two phases and is capable of being liquefied. In the in situ separ-
ation technique, a monomer is dissolved in the liquid vehicle and is then
subsequently polymerized at the interface. Deposition of the liquid poly-
mer coating around the core material is accomplished by controlled
physical mixing of the coating material (while liquid) and the core
material in the manufacturing vehicle in the liquid phase; this sorption
phenomenon is a prerequisite to effective coating. Continued deposition
of the coating is prompted by a reduction in the total free interfacial
energy of the system brought about by a decrease of the coating material
surface area during coalescence of the liquid polymer droplets. Finally,
solidification of the coating is achieved by thermal, cross-linking, or des-
olventization techniques and forms a self-sustaining microcapsule. The
microcapsules are usually collected by filtration or centrifugation,
washed with an appropriate solvent, and subsequently dried by standard
techniques such as spray- or fluidized-bed drying to yield free-flowing,
discrete particles.
[7]
A large numbers of coating materials have been evaluated for coacer-
vation microencapsulation but the most studied and well understood
coating system is probably the gelatin=gum acacia system. However,
other coating systems such as gliadin, heparin=gelatin, carrageenan,
chitosan, soy protein, polyvinyl alcohol, gelatin=carboxymethylcellulose,
B-lactoglobulin=gum acacia, and guar gum=dextran are also studied.
[89]
In recent years, modified coacervation processes have also been developed
that can overcome some of the problems encountered during a typical
gelatin=gum acacia complex coacervation process, especially when dealing
with food ingredients; for example, a room-temperature process for the
encapsulation of heat-sensitive ingredients such as volatile flavor oils.
[90]
In this process, the coating materials are mixed and then phase separation
(coacervation) is achieved by adjusting the pH. The newly formed coacer-
vate phase is allowed to separate and sediment, most of the supernatant
water is removed, and the flavor oil is then added to the mixture kept at
50
C and pH 7
and the reaction is carried out over 16 h, after which a hardened shell
of coacervate is formed around the flavor oil droplets.
[92]
Centrifugal Suspension Separation
Centrifugal suspension is more recent microencapsulation process. The
process in principle involves mixing the core and wall materials and then
adding to a rotating disk. The core materials then leave the disk with a
coating of residual liquid. The microcapsules are then dried or chilled
after removal from the disk. The whole process can take between a few
seconds to minutes. Solids, liquids, or suspensions of 30 mm to 2 mm
can be encapsulated in this manner. Coatings can be 1200 mm in thick-
ness and include fats, polyethylene glycol (PEG), diglycerides, and other
meltable substances. Since this is a continuous, high-speed method that
can coat particles, it is highly suitable for foods. One application is to
protect foods that are sensitive to or readily absorb moisture, such as
aspartame, vitamins, or methionine.
[93]
The preparation process of encap-
sulated particles by centrifugal suspension separation is illustrated in
Fig. 8.
Cocrystallization
Cocrystallization is a new encapsulation process utilizing sucrose as a
matrix for the incorporation of core materials. The sucrose syrup is con-
centrated to the supersaturated state and maintained at a temperature
high enough to prevent crystallization. A predetermined amount of core
material is then added to the concentrated syrup with vigorous mechanical
agitation, thus providing nucleation for the sucrose=ingredient mixture
to crystallize. As the syrup reaches the temperature at which transform-
ation and crystallization begin, a substantial amount of heat is emitted.
Agitation is continued in order to promote and extend transformation=
crystallization until the agglomerates are discharged from the vessel.
The encapsulated products are then dried to the desired moisture (if
necessary) and screened to a uniform size. It is very important to properly
control the rates of nucleation and crystallization as well as the thermal
balance during the various phases.
[94]
Microencapsulation of Food Ingredients 1381
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The advantages of this technique include: (1) It can be employed to
achieve particle drying. By means of this process, core materials in a
liquid form can be converted to a dry powdered form without additional
drying. (2) Products offer direct tableting characteristics because of their
agglomerated structure and thus offer significant advantages to the candy
and pharmaceutical industries. Recently, Beristain et al. encapsulated
orange peel oil by a cocrystallization technique.
[95]
In their study, encap-
sulation capacity of sucrose syrups was found to be greater than 90%for
a range of 100 to 250 g oil=kg of sugar. Surface oil, a measurement of
encapsulation efficiency, varied from 3350 to 8880 mg oil=kg solids.
Moisture content of the crystals was lower than 10 g=kg, and bulk density
was greater than 670 kg=m
3
for all the cocrystallizates prepared. Sensory
evaluation showed that all of the panelists were able to detect oxidized
flavors in oils without antioxidant added after storage at 35
C for one
day. When butylated hydroxyanisole was added to the oil prior to cocrys-
tallization, no signs of oxidized flavors were detected after 2 months of
storage at ambient temperature.
Liposome Entrapment
Liposomes consist of an aqueous phase that is completely surrounded by
a phospholipid-based membrane. When phospholipids, such as lecithin,
Figure 8. Representation of rotational suspension separation (A: establishing
particle size for pure coating, and B: encapsulation by suspension separation).
1382 Desai and Park
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are dispersed in an aqueous phase, the liposomes form spontaneously.
One can have either aqueous or lipid-soluble material enclosed in the
liposome. They have been used for delivery of vaccines, hormones,
enzymes, and vitamins.
[96]
They consist of one or more layers of lipids
and thus are nontoxic and acceptable for foods. Permeability, stability,
surface activity, and affinity can be varied through size and lipid compo-
sition variations. They can range from 25 nm to several microns in diam-
eter, are easy to make, and can be stored by freeze-drying. Kirby and
Gregoriadis have devised a method to encapsulate at high efficiency,
which is easy to scale-up and uses mild conditions appropriate for
enzymes.
[97]
It is important to reiterate that large unilamellar vesicles
(LUV) are the most appropriate liposomes for the food industry because
of their high encapsulation efficiency, their simple production methods,
and their good stability over time. The great advantage of liposomes over
other microencapsulation technologies is the stability liposomes impart
to water-soluble material in high water activity application: spray-dryers,
extruders, and fluidized beds impart great stability to food ingredients in
the dry state but release their content readily in high water activity appli-
cation, giving up all protection properties. Another unique property of
liposomes is the targeted delivery of their content in specific parts of the
foodstuff. For example, it has been shown that liposome-encapsulated
enzymes concentrate preferably in the curd during cheese formation,
whereas nonencapsulated enzymes are usually distributed evenly in the
whole milk mixture, which leads to very low (24%) retention of the
flavor-producing enzymes in the curd. They have prepared bromelain-
loaded liposomes for use as meat-tenderizer to improve stability of
the enzyme during the processing of the food and subsequently improve
the availability of the enzyme.
[98]
Benech Kheadr et al. showed that
liposome-entrapped nisin retained higher activity against Listeria inno-
cua and had improved stability in cheese production, proving a power-
ful tool to inhibit the growth of Listeria I in cheese while not preventing
the detrimental effect of nisin on the actual cheese-ripening process.
[99]
Kirby et al. have developed a process to stabilize vitamin C in the aque-
ous inner core of liposomes.
[100]
Encapsulation of vitamin C gave sig-
nificant improvements in shelf life (from a few days to up to 2 months),
especially in the presence of common food components that would nor-
mally speed up decomposition, such as copper ions, ascorbate oxidase,
and lysine. Liposomes can also be used to deliver the encapsulated
ingredient at a specific and well-defined temperature: the liposome
bilayer is instantly broken down at the transition temperature of the
phospholipids, typically around 50