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12/15/2014

การพัฒนากระบวนการกักเก็บกลิน่ และ
รสชาติของเครื่ องเทศสมุนไพรไทย
ผศ.ดร.อภินันท์ สุ ทธิธารธวัช
ศูนย์เชี่ยวชาญเทคโนโลยีอนุภาค ภาควิชาวิศวกรรมเคมี
จุฬาลงกรณ์มหาวิทยาลัย
Email: apinan.s@chula.ac.th

Encapsulation Technology Encapsulation Technology

• Encapsulation can be defined as a process where • Encapsulation technology has been used in the
a continuous thin coating is formed around solid food industry for more than 60 years as a way to
particles, liquid droplets, or gas cells that are fully provide liquid and solid ingredients as an effective
contained within the capsule wall (King, 1995). barrier for environmental and/or chemical
• Encapsulation is a topic of interest in a wide range interactions until release is desired (Reineccius,
of scientific and industrial areas, varying from 1994).
pharmaceutics to agriculture and from pesticides to
enzymes.

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Encapsulation Technology Morphology of microcapsule


Approximate 60 years ago, encapsulation processes were
developed. It involves the coating and entrapment of a pure
material or mixture into another material. The coated or entrapped
material is usually a liquid but can be a solid or gas. Natural
examples include birds’ egg shells, plant seeds, bacterial spores,
skin and seashells.
Core material
Wall
Core Active Shell

Wall material/ capsule

Its Advantages Its Advantages

1. Reduce the reactivity of the core with regard to 4. Promote the ease of handling of the core material.
the outside environment, for example oxygen and 5. Mask the taste of the core.
water. 6. Dilute the core material when it is only used in
2. Decrease the evaporation or transfer rate of the very small amounts; but, achieve uniform
core material with regard to the outside dispersion in the host material.
environment.
3. Control the release of the core material so as to
achieve the proper delay until the right stimulus.

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Criteria to be aware Criteria to be aware

• Microcapsule properties may be changed to suit • Furthermore, the different processing conditions
specific core applications, including composition, that the product will go through before release are
mechanism of release, particle size, final physical of essential consideration.
form, and cost. • Other important features to take into account are
• When designing encapsulation processes, it must the optimum concentration of the active core, the
be clearly established what type of functions mechanism of release, the final particle size,
encapsulated core can provide to the final product density, and stability requirements of the
in order to select the most suitable coating encapsulated ingredient.
material.

Type of capsule by their size Types of Encapsulated Ingredients


Various food ingredients that can be encapsulated (adapted from
• Encapsulated particles are called microcapsules Gibbs et al., 1999).
when the size range is between 0.2 and 5,000 μm. - Flavoring agents - Preservatives
• Macrocapsules when the range is larger than - Acids, akalis, buffers - Colorants
5,000 μm. - Lipids - Cross-linking and setting
- Redox agents (bleaching, agents
• Nanocapsules when the range is smaller than 0.2 maturing) - Agents with undesirable
μm (200 nm) (King, 1995). - Enzymes and flavor and odors
microorganisms - Essential oils, amino
- Artificial sweeteners acids, vitamins, minerals
- Leavening agents

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Coating/ Wall materials Coating/ Wall materials


A summary of typically used coating material in food industries For Food Industry
(adapted from Greenblatt et al., 1993; Shahidi and Han, 1993).

Technique for encapsulation Microcapsule


Various techniques are used for encapsulation. In general, the
main process composed of formation of the wall around the material, Particle size ranges for selected encapsulation methods (adapted
from Vasishtha, 2002).
ensuring that leakage does not occur, and ensuring that undesired
materials are kept out. These encapsulation techniques include:

 Spray drying  Liposome entrapment


 Spray chilling  Coacervation,
 Spray cooling  Inclusion complexation
 Extrusion coating  Centrifugal extrusion
 Fluidized bed coating  Rotational suspension separation
 Co-crystallization  Interfacial polymerization

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Overview of common process Overview of common process

Overview of common process Overview of common process

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Overview of common process Process to encapsulate flavors


Various encapsulated methods have been proposed. Among them,
spray drying is the most common technique to produce flavor
powders from food flavor emulsion.

Flavor
Spray drying

10 m Flavor

Flavor emulsion (Liquid state) Encapsulated flavor powder (Solid state)

How to make the encapsulation of flavors? How to make the encapsulation of flavors?
2. Spray drying
1. Preparation of emulsion Atomizer
The emulsion is then fed into the spray dryer Cyclone
First the hydrophobic flavors should be emulsified in the carrier and transformed into droplets by an atomizer.
solution to create the flavor emulsion. Carrier solution normally The hot air flowing contacts the atomized
compose of emulsifier and additive wall materials. particles and evaporates the water. The dried Product
Vessel
particles, consisting of dry matrices in which
Emulsions are heterogeneous systems Emulsion size Carrier the core material, is held in a micro
which consists of two immiscible solution dispersion.
liquids (usually oil and water) with
Emulsion
Spray drying is by definition the Drying
one of the liquids dispersed in another Chamb
droplet transformation of a feed of liquid or paste Blowe
as small spherical droplets. er
material (solution, dispersion or paste) into a r

dried particulate powder by spraying the feed


into a hot drying medium.

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Flavor retaining mechanism Factor influencing the flavor retention


Carrier solution Explained by the “Selective Diffusion 1. Properties of volatile compounds
Atomization - Molecular weight
period Flavor emulsion
Theory” (Thijissen, 1968). As the
water concentration at the droplet - Vapor pressure
Water evaporation surface decreases, the diffusion - Solubility
Crust formation coefficients of the volatile components
Evaporatio 2. Properties of the emulsion/feed solution
n period decrease by several orders of - Solid Concentration
Selective diffusion
of flavor magnitude, more sharply than that of - Viscosity
Water evaporation water. The dry surface acts as a semi-
Morphology - Emulsion size
Selective diffusion permeable membrane permitting the
Change period of flavor - Emulsion stability
continued loss (or diffusion) of water,
- Concentration of flavor in the emulsion
but efficiently retaining (or stopping)
Spray-dried
volatile flavor. - Additive materials
powder
- Infeed temperature

Factor influencing the flavor retention Factor influencing the flavor retention

3. Type of capsule wall material 4. Drying process conditions


- Mono- and disaccharides - Atomization: Type and particle size

- Hydrolyzed starches - Atomized droplet size


- Chemically modified starches - Dryer inlet temperature

- Gums - Dryer outlet air temperature

- Proteins (soybean) - Drying air velocity/ Air flows in the spray dryer

- Blend of Gum arabic and hydrolyzed starch - Humidity of the dryer inlet air

- Blend of modified starches and maltodextrin


- Blend of hydrolyzed starches with proteins and lipids

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High content of lemongrass oil powder Microencapsulation of multi-flavor compounds


process by spray drying
Research Core Technologies: Process, wall/core materials Research Core Technologies: Process, wall/core materials
Product: High content of encapsulated lemongrass powder Product: Encapsulated multi flavors powder
Target applications: Seasoning powder/ antibacterial powder Target applications: Seasoning powder/ antibacterial powder

Spray drying

Spray drying

Extracted lemongrass
40 wt% of lemongrass oil Extracted bergamot oil

Encapsulation of lemongrass oil with cyclodextrins


by spray drying
Research Core Technologies: Process, wall/core materials
Product: Lemongrass oil inclusion complex
Target applications: Antibacterial powder

Extracted lemongrass 2kV x 250                                    10m Encapsulation of Bergamot


Spray drying
and lemon grass oil by
spray drying

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Targets/Objective of the work Extracted lemongrass oil

Capsules of lemongrass oil and bergamot oil Citral (3,7-dimethyl-2,6-octadienal)


for development in instant Tom Yum soup
product up to originality. C10H16O
Increase the lemongrass oil content in the O
capsule comparing to the conventional
method  Major component in lemongrass oil
 High susceptible to acid-promoted
Use data based on this research as
 High oxidative degradation
a reference for food industries.  Anti-bacterial properties

The encapsulation should improve their stability.

Extracted bergamot oil Gum arabic


• Linalool 16%
• Linalyl acetate 32% • Gum arabic is a complex mixture of
• Limonene 38% polysaccharides and glycoproteins that is
used primarily in the food industry as a
stabilizer.

Linalyl Acetate (an Limonene Linalool (an alcohol)


ester) b.p. 178 °C b.p. 198 °C
b.p. 220 °C 35
Introduct
i

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Modified starch Objectives


Feature HI-CAP 100 CAPSUL Prove the assumption that the small feed emulsion size
Description Chemically modified* Chemically modified* will increase the oil contents in the final product.
food starch refined from food starch refined from Determination of  suitable carrier material
waxy maize waxy maize
 condition of emulsification process
Appearance Fine white powder Fine off-white creamy
 condition of spray drying process
powder
 moisture content
Surface properties Hydrophilic and Hydrophilic and
hydrophobic hydrophobic  surface oil
Structure Unique polymer Unique branched
By Characterize  flavor retention
polymer  particle size
 morphology
*Note: “chemically modified” means an n-octenyl succinic
anhydride (OSA)-modified starch blended with corn syrup solids.

Preparation of flavor emulsion


Wall material
Feed liquid
Homogenizing Spray drying Spray-dried powder
emulsion
Flavor
solid content : 50%
wall material : Capsul
(Modified starch), Acacia
Gum+ Maltodextrin (1:3)

Experimental Methods flavor : lemongrass oil


Concentration 20, 40, 50, 60,
80 %w/w of total solid
homogenization :
8000 rpm 3 min

emulsion size : SALD

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Emulsification method Preparation of spray-dried powder


Wall material
Feed liquid
Homogenizing Spray drying Spray-dried powder
emulsion
Flavor
High Speed  air inlet temperature : 160ºC
Homogenizer 8000 rpm
 speed of atomizer : 30,000 rpm
 feed rate : 30 ml/min
 air flow rate : 110 kg/hr
Avestin Microfluidic

Cycle : 1, 3, 5 • surface oil : GC 2010


• flavor retention : GC 2010
Pressure(psia) : 500, 1000, 1500
• particle size : SALD
• morphology : SEM
• water content : KF titrator

Spray Dryer Flavor Retention


water 2 ml acetone 4 ml

extract at 90 ºC
30 min
vortex mixer 1 min
powder 0.1 g
1 µl
Condition of GC
centrifugation
Type : 2010 3,000 rpm 10 min
Column : DB-WAX
INJ Temp : 210 oC
Buchi, DET Temp : 230 oC (FID)
Gear Niro Ohkawara L-8 Inlet Press : 70 kPa
Model B-290 Mobile Minor

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Surface Oil measurements


hexane 1 ml

powder 0.1 g

A B C D
Experimental Results
1 µl

Effect of Oil contents


5 times 10 times 15 times 20 times
(Lemongrass Oil)

Effect of oil loading on emulsion size Effect of oil loading on emulsion size
3.5 Modified Starch: Capsul GA+MD
30 30
D43 of flavor in feed emulsion (m)

20 wt%
3.0 40 wt%
25 50 wt% 25
GA+MD
2.5 60 wt%

Volume fraction (%)

Volume fraction (%)


20 80 wt% 20
2.0
15 15
1.5
10 10
1.0 Modified Starch: Capsul
5 5
0.5
0 0
0
0 20 40 60 80 100 0.1 1 10 0.1 1 10
Oil concentration (%wt of total solid) Diameter (m) Diameter (m)

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Effect of oil loading on re-constitute Effect of oil loading on retention and water
emulsion and powder size content
Modified Starch: Capsul GA+MD Flavor Retention Water Content
1.0 4
D43 of flavor in feed emulsion (m)

100

D43 of flavor in feed emulsion (m)

Water content (% wt of powder)


Modified Starch: Capsul 8
0.8 Feed Emulsion 80

Citral Retention (%)


3 GA+MD
Feed Emulsion 6
0.6 60
2
4
0.4 40

1 2
0.2 Reconstitute Emulsion Reconstitute Emulsion 20
GA+MD Modified Starch: Capsul

0 0 0 0
0 20 40 60 80 100 0 20 40 60 80 100 0 20 40 60 80 100 0 20 40 60 80 100
Oil concentration (%wt of total solid) Oil concentration (%wt of total solid) Oil concentration (%wt of total solid) Oil concentration (%wt of total solid)

Effect of oil loading on encapsulated oil Effect of oil loading on encapsulated


and surface oil content oil without surface oil (after washed)
100
Modified Starch: Capsul

Encapsulated citral content after


40
X=Y
Surface oil (% wt of powder)

30

washing (% of total powder)


Encapsulated citral content

80
(% of total powder)

30
60 Modified Starch: Capsul
20
GA+MD
20
40

10 GA+MD
10 20

0 0 0
0 20 40 60 80 100 0 20 40 60 80 100 0 20 40 60 80 100
Oil concentration (%wt of total solid) Oil concentration (%wt of total solid) Oil concentration (%wt of total solid)

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Effect of oil loading on the external Effect of oil loading on the internal
morphology morphology
Initial Oil concentration (%wt of total solid) Initial Oil concentration (%wt of total solid)
Modified Starch: Capsul Modified Starch: Capsul
20 % wt 40 % wt 50 % wt 60 % wt 80 % wt 20 % wt 40 % wt 50 % wt 60 % wt 80 % wt
b

X 400 50µm X 400 50µm X 400 50µm X 400 50µm X 400 50µm X 2,500 10µm X 2,500 10µm X 2,500 10µm X 2,500 10µm X 2,500 10µm

b c c

X 2,000 10µm X 2,000 10µm X 2,000 10µm X 2,000 10µm X 2,000 10µm X 6,500 2µm X 6,500 2µm X 6,500 2µm X 6,500 2µm X 6,500 2µm
Oil concentration Oil concentration Oil concentration Oil concentration Oil concentration
20 % Dry basis 38.3 % Dry basis 41.9 % Dry basis 46.1 % Dry basis 51.2 % Dry basis

Effect of oil loading on the external Effect of oil loading on the internal
morphology morphology
Initial Oil concentration (%wt of total solid) Initial Oil concentration (%wt of total solid)
Agacia Gum + Malto dextrin 1:3 Agacia Gum + Malto dextrin 1:3
20 % wt 40 % wt 60 % wt 20 % wt 40 % wt 60 % wt
b

X 400 50µm X 400 50µm X 400 50µm

X 2,000 10µm X 2,000 10µm X 2,000 10µm


Oil concentration Oil concentration Oil concentration
15.7 % Dry basis 30.6 % Dry basis 33.0 % Dry basis

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Preparation of flavor powder


Wall material
Feed liquid
Homogenizing Spray drying Spray-dried powder
emulsion
Flavor
 air inlet temperature : 160 ºC
solid content : 40%
 speed of atomizer : 30,000 rpm
wall material : Capsul

Experimental Results flavor : lemongrass oil


40 % of total solid
 feed rate : 30 ml/min
 air flow rate : 110 kg/hr

Effect of emulsion size


(Lemongrass Oil) emulsion size : SALD • flavor retention : GC 2010
• particle size : SALD
• morphology : SEM

Emulsification process to Effect of emulsion size on retention and


control emulsion size surface oil content
40
100 10

Surface oil content (% wt of powder)


Mean emulsion
Condition size (µm) 30 80 8
Volume fraction (%)

Citral Retention (%)


A. 8000 rpm 3 min 0.29 B C
A 60 6
B. 6000 rpm 1 min 0.61 20

C. 4000 rpm 4 min 0.83 D 40 4


D. 3000 rpm 2 min 1.16 10

20 2
0
0.1 1 0 0
0 0.5 1.0 1.5 2.0 0 0.5 1.0 1.5 2.0
Diameter (m)
Emulsion size (m) Emulsion size (m)

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Effect of emulsion size on the Effect of emulsion size on the


external morphology internal morphology
8000 rpm 3 min (0.29 m) 4000 rpm 4 min (0.83 m) 8000 rpm 3 min (0.29 m) 4000 rpm 4 min (0.83 m)

X 400 50µm X 2,000 10µm X 400 50µm X 2,000 10µm X 2,500 10µm X 6,500 2µm X 2,500 10µm X 6,500 2µm

6000 rpm 1 min (0.61 m) 3000 rpm 2 min (1.16 m) 6000 rpm 1 min (0.61 m) 3000 rpm 2 min (1.16 m)

X 2,000 10µm X 2,500 10µm X 6,500 2µm X 2,500 10µm X 6,500 2µm
X 400 50µm X 2,000 10µm X 400 50µm

Preparation of flavor emulsion


Wall material
Feed liquid
Homogenizing Spray drying Spray-dried powder
emulsion
Flavor

solid content : 50%  air inlet temperature :


wall material : Capsul 120 140 160 and 180ºC

Experimental Results
flavor : lemongrass oil  speed of atomizer : 30,000 rpm
concentration 40 % of
total solid  feed rate : 30 ml/min
homogenization :  air flow rate : 110 kg/hr

Effect of air inlet temperature 8000 rpm 3 min

• flavor retention : GC 2010


(Lemongrass Oil) • particle size : SALD
emulsion size : SALD • morphology : SEM

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Effect of inlet air temperature on the


Effect of inlet air temperature on powder size retention and surface content
50 25 3.0
D43 of flavor in feed emulsion (m)

100 3.0

Water content (% wt of powder)


Surface oil (% wt of powder)
40 20 160 C 2.5
2.5

Volume fraction (%)

Citral Retention (%)


180 C 90
2.0
30 15 120 C 2.0
80
1.5
10 140 C 1.5
20
70
1.0
1.0
5
10 60 0.5 0.5
0
0 50 0 0
120 140 160 180 10 100 120 140 160 180 120 140 160 180
Inlet air temperature (C) Diameter (m) Inlet air temperature (C) Inlet air temperature (C)

Effect of inlet temperature on the Effect of inlet temperature on the


external morphology internal morphology
120 ºC 160 ºC 120 ºC 160 ºC

X 400 50µm X 2,000 10µm X 400 50µm X 2,000 10µm X 2,500 10µm X 6,500 2µm X 2,500 10µm X 6,500 2µm

140 ºC 180 ºC 140 ºC 180 ºC

X 400 50µm X 2,000 10µm X 400 50µm X 2,000 10µm X 2,500 10µm X 6,500 2µm X 2,500 10µm X 6,500 2µm

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Effect of inlet temperature on the Effect of inlet temperature on the


internal morphology: 120 C internal morphology: 140 C

Effect of inlet temperature on the Effect of inlet temperature on the


internal morphology: 160 C internal morphology: 180 C

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Conclusion and Remarks


• The high content of lemongrass oil powder (higher
than 40 % w/w) could be successfully prepared in
the modified starch materials with low surface oil
content. Comparing to 20 % w/w of conventional
materials.
• The encapsulation efficiency and oil content in the
final powder could be improved by decreasing the
oil emulsion size.
Experimental Results
• The operating of air drying condition did not show
much effect on the retention of flavor but the Multi-flavor extracted oil
morphology, thickness of wall, was observed to
change with the air drying temperature. (Bergamot Oil)

Flavor retention Relative content of flavor


100 58
95.25 98.5 57 59
87.34 50 57
87.86 60

Relative content
100
Flavor retention(%)

75.14 66.04 50
76.25
80 40
62.72 67.56 55.05 28 22 22 23
60 30 22 23
Linalyl acetate 19 20
47.95 20 18 20 linalyl acetate
40
Limonene 10 linalool
20 Linalool 0
limonene
0 Main component Percentage(%)
HI-CAP Linalool 17.08
(1:8) HI-CAP
(1:4) CAPSUL
CAPSUL Linalyl acetate 22.33
(1:8)
(1:4) Limonene 40.28
Higher wall material content increased the rate of
formation of semipermeable membrane resulting in
the reduction of flavor loss during spray drying.

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Cyclodextrins
Cyclodextrins are produced in
technical plants by enzymatically
catalyzed degradation of starch.

Glucopyranose unit[2] Doughnut shaped

ENCAPSULATION OF
Chemical structures[3] ring structure[2]

LEMONGRASS OIL WITH CD CD CD

CYCLODEXTRINS BY
SPRAY DRYING
[2] Jafari, S.M., Assadpoor, E., He, Y. and Bhandari, B., Encapsulation Efficiency of Food Flavours and Oils during Spray Drying. Drying Technology. 26; 816–835 (2008)
[3] Venturinii, C.G., Nicolini , J. and Machado, C.,PROPRIEDADES E APLICAÇÕES RECENTES DAS CICLODEXTRINAS . Quim. Nova. 31(2) 360-368 (2008)

Cyclodextrins Preparation of inclusion complexes

Cyclodextrins slurry  
(10, 20, 30 wt%) 

 Lemongrass oil  
(Citral:CD molar ratio = 1:1)  

Shaking at 45C  
for 12 h Drying conditions
Model Spray Dryer B‐290, BUCHI 
Nozzle Two ‐fluid nozzle ( = 0.5)
Spray drying  Inlet temp (C) 160
Feed rate (mL/min) 9
Gas flow rate (m3/h) 38

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‐CD ‐CD ‐CD


Preparation of inclusion complexes
CHO
 Feed liquid  CHO CHO CHO
Cyclodextrins slurry   Pump                   
(20 wt%)  Atomizer  1 nm

Heater 
 Lemongrass oil  
(Citral:CD molar ratio = 1:1, 1.5:1, 2:1)   Exhaust                    E‐citral
Inlet Air 
0.6 nm

Drying Chamber  Outlet Air  Cyclone 


Shaking at 45C for 12 h
Collector 
1 nm
Drying conditions CHO CHO CHO
Homogenized at 8000 rpm 
Model Ohkawara Type L‐8 Spray Dryer  CHO
for 3 min 
Nozzle Rotary nozzle
Atomizer speed (rpm) 30,000 Z‐citral
Spray drying  Inlet temperature (C) 160
Air flow rate (kg/h) 110 ‐CD ‐CD   ‐CD 
Feed flow rate  (mL/min) 30 Inner cavity  0.57 nm 0.78 nm 0.95 nm

Effect of citral/CDs molar ratio on 
morphology Preparation of inclusion complexes
 Feed liquid 
Native ‐CD  1:1 
Cyclodextrins slurry  
Pump                   
(20 wt%) 
Atomizer 

 Lemongrass oil   Heater 
(Citral:CD molar ratio = 1:1)  
Exhaust                   
Inlet Air 
Shaking at 45C for 12 h
2kV x 250                                    10m 2kV x 250                                    10m Drying Chamber  Outlet Air  Cyclone 
Added maltodextrin  Collector 
1.5:1  2:1  (MD, DE=25)
Drying conditions
Model Ohkawara Type L‐8 Spray Dryer 
Homogenized at 8000 rpm 
for 3 min  Nozzle Rotary nozzle
Atomizer speed (rpm) 30,000
Inlet temperature (C) 160
Air flow rate (kg/h) 110
Spray drying 
2kV x 250                                    10m 2kV x 250                                    10m Feed flow rate  (mL/min) 30

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Effect of MD on morphology Effect of MD on morphology
‐CD 100%  ‐CD 80% + MD 20%  ‐CD 100%  ‐CD 80% + MD 20% 

2kV x 250                                    100m 2kV x 250                                    100m 2kV x 250                                    10m 2kV x 250                                    10m

‐CD 60% + MD 40%  ‐CD 20% + MD 80%  ‐CD 60% + MD 40%  ‐CD 20% + MD 80% 

2kV x 250                                    100m 2kV x 250                                    100m 2kV x 250                                    10m 2kV x 250                                    10m

Effect of MD on morphology Effect of MD on morphology
‐CD 100%  ‐CD 80% + MD 20%  ‐CD 100%  ‐CD 80% + MD 20% 

2kV x 250                                    100m 2kV x 250                                    100m 2kV x 250                                    10m 2kV x 250                                    10m

‐CD 60% + MD 40%  ‐CD 60% + MD 40% 

2kV x 250                                    100m 2kV x 250                                    10m

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Encapsulation of Citronella Oil in Starch-Based


Aggregates by Spray Drying
Effect of MD on total oil retention Research Core Technologies: Process, wall/core materials
Product: Encapsulated citronella in aggregates starch powder
‐CD ‐CD Target applications: Mosequitoes-replelling body powder

Spray drying
Native rice starch
, E‐citral   , Z‐citral

Retention : 
‐The combined CDs and MD encapsulant does not affect the total citral 
retention but release rate due to the film formation in the presence of 
MD. 
Citronella oil

Preparation of fish sauce powder by Spray Drying High quality honey powder
Research Core Technologies: Process, wall/core materials
Research Core Technologies: Process, wall/core materials Product: High content of honey powder
Product: Encapsulated fish sauce powder Target applications: Seasoning powder
Target applications: Seasoning powder

Spray drying

MD + GA
Spray drying

Fish sauce
MD + Gelatin

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Development of Redispersible Dry Nanoemulsion Encapsulation of Phytase by Spray drying


for Water-insoluble Drug Delivery
Research Core Technologies: Process, wall/core materials Research Core Technologies: Process, wall/core materials
Product: Dried nanoemulsion Product: Targeted release of encapsulated phytase powder
Target applications: Drug delivery Target applications: Animal supplement feed

Spray drying

Encapsulation of Phytase by Spray drying Encapsulation of multi-enzymes by spray drying


Research Core Technologies: Process, wall/core materials
Product: Ecapsulated multi-enzymes powder
Target applications: Animal supplement feed

Multi-Enzymes

Cellulase Xylanase Spray drying


DE10

Cellulose Hemicellulose
DE17

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Microencapsulation process steps


Operating condition
(Shahidi and Han(1993)
• Main factor
1. Preparation of the dispersion or emulsion 1. Feed temperature
2. Homogenization of the dispersion
3. Atomization of the infeed emulsion Feed temperature Viscosity and droplets size
↑ ↓
4. Dehydration of the atomized particles
But high temperatures can cause
volatilization or degradation of
some heat-sensitive ingredients.

Operating condition Operating condition

2. Air inlet temperature 3. Air outlet temperature


• It is directly proportional to the microcapsule • It is quite difficult to predict this outlet temperature in
drying rate and the final water content. advance for a given product, since it depends on the
drying characteristics of the material.
High density membranes, high
Air inlet temperature ↓ water content, agglomeration • The air outlet temperature cannot be directly controlled
since it depends on the air inlet temperature.
• The ideal air outlet temperature for the
microencapsulation of food ingredients such as flavors
Air inlet temperature ↑ Crack in the membrane has been reported to be 50-80℃.
(excessive evaporation) inducing subsequent
premature release.

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Experimental conditions recently optimized for the 5. Microencapsulation by spray-


encapsulation of some different food ingredients by
spray-drying
drying: which wall must be used ?

• Wall material required properties


• Wall material selection
• Most commonly used wall materials

Wall material required properties Wall material selection


Type 1 : maltodextrin,
• The wall materials must be soluble in water at an pullulan, gum arabic and
gelatin
acceptable level. (Gouin, 2004)
• Good properties of emulsification, film forming, Type 2 : sodium
and drying. (Reineccius, 1988) caseinate and albunim

• The wall concentrated solutions should have low


viscosity. (Reineccius, 1988) Type 3 : glucose

Type 4 : mannitol

Schematic characteristic isothermal drying curves of various wall materials. See text for
details. (Matsuno & Adachi, 1993).

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Most commonly used wall materials Literature


• Carbohydrates such as starches, maltodextrins and corn
• Maltodextrins provide good oxidative stability to
syrup solids are usually used in microencapsulation of encapsulated oil but exhibit poor emulsifying capacity,
food ingredients. (Dezarn, 1995; Kenyon, 1995) emulsion stability and low oil retention. (Kenyon, 1995)
• The retention of emulsified ethyl butyrate during spray-
PIC drying was shown to be dependent on the maltodextrin
PIC concentration and type of emulsifier. (Yoshii et al., 2001)
starches
maltodext • The maltrodextrins with dextrose equivalence between 10
and 20 fit in for using as wall material. They show the
rin highest retention of flavor because they could be
dispersed in water up to 35.5% of the solution without
Because they exhibit low viscosities at high solids contents and good haze formation. (Raja et al., 1989)
solubility, but most of them lack the interfacial properties requires for • A pectin content of 1-2% is considered to be sufficient for
high microencapsulation efficiency and generally associated with the preparation of a stable emulsion for spray drying.
other encapsulating materials such as proteins or gums. (Drusch, 2006)

Most commonly used wall


Literature
materials
• Gums are used in microencaapsulation for both their film forming
Gum arabic was found to be a better wall
and emulsion stabilization properties. material for encapsulation of cardamom
oleoresin than maltodextrins and modified
• Such as gums, acacia gum, gum arabic. starch and the obtained microcapsules
exhibited a free flowing character. (Krishnan et
PIC al., 2005)
The partial replacement (50%) of gum arabic
gum with glucose was reported to increase
microencapsulation efficiency of soy oil from
74% to 92%. (McNamee et al., 2001)

Gum arabic was not efficient as a wall material for the encapsulation of five different
monoterpenes (citral, linalool, β-myrcene, limonene, and β-pinene). (Bertolini et al.,
2001)

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Most commonly used wall materials Literature


• Whey proteins have been successfully used as a wall system to
• Protein encapsulate anhydrous milk fat by spray-drying and
encapsulation yield greater than 90% was obtained. (Young et al.,
• The most commonly used proteins for 1993)
encapsulating food ingredients by spray-drying • Caraway essential oil could be encapsulated in a wall system
consisting of milk proteins which should provide it an effective
are milk or whey proteins and gelatin. protection against oxidation. (Bylaite et al., 2001)
• Small amount (1%(w/w)) of gelatin could increase the retention of
ethyl butyrate when gum arabic is used as emulsifier and
according to (Yoshii et al., 2001), the early formation of the surface
crust due to the presence of gelatin, prevented the loss of ethyl
butyrate emerged from the unstable ethyl butyrate emulsion.

Thank you for your


attention

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