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Microencapsulation Methods Physical Processes
CSIRO FOOD AND NUTRITION
Luz Sanguansri & MaryAnn Augustin
Short Course on Micro- and Nano-encapsulation of Functional Ingredients in Food Products World Congress on Oils & Fats and 31st Lectureship Series 31st Oct – 4th November 2015, Rosario, Argentina
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Outline
• Microencapsulation Processes
• Considerations for method selection
• 5-Step process
• Encapsulant preparation
• Core incorporation
• Core dispersion or homogenisation
• Particle or droplet formation
• Matrix or shell hardening and stabilisation
• Summary
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Microencapsulation processes used for food ingredients application
3 |
Physical Processes Chemical Processes
Spray drying Simple coacervation
Spray chilling Complex coacervation
Fluid bed coating Interfacial polymerisation
Spinning disk coating Liposome encapsulation
Co-extrusion Chemical adsorbents
Carbohydrate (melt) extrusion Inclusion complexation
Screw extrusion Thermal & ionic gelation
Sanguansri & Augustin | CSIRO
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Some considerations for process selection
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Beadlet | Hydrogel
Technology
•Thermal gelation
•Ionic gelation
•Enzymatic gelation
•Interfacial polymerisation
•Coacervation
Powder Technology
•Spray drying
•Spray-freezing
•Spray cooling (in melt solution)
•Spray chilling (in thermogel solution)
•Impinging aerosol method
Other processes
Extrusion (solid matrix)
•spheronisation
•pellets
Emulsification (liquid)
•Primary emulsion
•Double emulsion
Multiwall protection | double encapsulation
Fluid bed coating, layering and spray granulation
Application of additional coating layers (polymer coat or lipid coat) to primary microcapsules
Multi-stage stabilisation:
stabilisation techniques, microencapsulation, thermal adaptation, and protectant addition
Process chosen must be scalable and cost effective
…based on microcapsule format
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…based on size and morphology
6 | http://www.particlesciences.com/images/tb/Encapsulation-table1.jpg Sanguansri & Augustin | CSIRO
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…based on structure and morphology
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How do you choose which technology or process to use?
• The choice of microencapsulation method depends on…
• Properties of the core (liquid, solid, volatile)
• Requirements in the target food application
• Encapsulant material chosen
8 |
core
wall material
Sanguansri & Augustin | CSIRO
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What do I need to know beforehand?
• Active (core): liquid/solid, hydrophilic/hydrophobic, volatile/labile
• Target application: food/feed, dry/moist/liquid, country
• Type of capsule: size, dry/wet, powder/pellets/granules
• Production: volume, batch/continuous, on-site/sub-contractor
• Storage: dry/wet, temperature, shelf life, packaging
• Further processing: process condition, point of addition
• Release: solubilisation, temperature, shear, pressure, breakage
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Microencapsulation process
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Microencapsulation Process – 5 Steps
1. Encapsulant (material) preparation
2. Core preparation and incorporation
3. Core dispersion and homogenisation
4. Particle/droplet formation
5. Matrix/shell hardening or stabilisation
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Encapsulant preparation and core dispersion
Lipid / FatEncapsulant
Heat Disperse /
Homogenise
Encapsulant
melted
Solid Core
added
Dispersion
WaterEncapsulant
Solution
“Heat Disperse /
Homogenise
Encapsulant
materials added
Liquid Core
added
Emulsion
Oil core in aqueous solution Solid core in lipid melt
Encapsulant preparation
Core incorporation
Core dispersion
Particle formation
Matrix or shell stabilisation
homogenise homogenise
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Dispersion & Homogenisation systems…
Batch system Continuous system
Emulsion systems
Core Dispersed phase
Encapsulant Continuous phase
Encapsulant preparation
Core incorporation
Core dispersion
Particle formation
Matrix or shell stabilisation
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Dripping technologies
Poncelet (2011)
Encapsulant preparation
Core incorporation
Core dispersion
Particle formation
Matrix or shell stabilisation
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Spray/atomisation technologies
Poncelet (2011)
Encapsulant preparation
Core incorporation
Core dispersion or homogenisation
Particle or droplet
formation
Matrix or shell hardening and
stabilisation
Atomisation of liquid droplets in air
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Spray Drying
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Spray drying
Burgain et al 2011, Food Eng
formulation is atomized as
droplets
Solution, suspension, dispersion,
emulsion with added bioactive
Spray dried microcapsules
Schematic presentation of the spray-drying procedure
Encapsulant preparation
Core incorporation
Core dispersion or homogenisation
Particle or droplet
formation
Matrix or shell hardening and
stabilisation
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Omega-3 oil encapsulation (example)
Water Encapsulant
Solution
Spray Drying
Chamber
Cyclone
Separator
Hot Air
Microencapsulated
Powder
Feed to the dryer
Heat Homogenise
Encapsulant
materials added Oil Core
added
Encapsulant preparation
Core incorporation
Core Dispersion or homogenisation
Particle or Droplet
formation
Matrix or shell hardening and
stabilisation
Emulsion preparation Spray Drying
Emulsion - droplets Size: 0.2-10 µm Powder - particles Size: 30-100 µm
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Probiotic encapsulation (example)
Encapsulant preparation
Core incorporation
Core Dispersion or homogenisation
Particle or Droplet
formation
Matrix or shell hardening and
stabilisation
Suspension preparation Spray Drying
Probiotic suspension Size: 5-10 µm Powder - particles Size: 30-100 µm
Water
Microcapsule
Probiotics(LGG)
Encapsulant matrix
Protein RS Starch
Protein + CHO Solution
Spray Drying Chamber
Cyclone Separator
Hot Air
Microencapsulated Powder
Probiotic +Encapsulant
Mixture
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Spray drying
• Most common process to convert liquid to powder
• Spray aqueous solution/dispersion in hot air
• Large throughput - capacity several tones per hour
• Produce free flowing, fine to granulated powders
• Low thermal effect on materials during drying
• Versatile and readily available in the food industry
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Spray Drying
Factors affecting microcapsule properties • Feed to the dryer
– Core type and payload
– Stability of the core and the emulsion/dispersion
– Total solids and viscosity of the feed
– Encapsulant material
• Process conditions – Homogenization
– Atomization
– Drying temperature (inlet and outlet)
– Air flow (co-current / counter-current)
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Spray Drying
Application
• Conversion of liquid ingredients in aqueous solution or dispersions
• Microencapsulation of flavors, vitamins, minerals, probiotics, enzymes, colors, acidulants, food additives, lipids, lipid soluble bioactives, extracts, etc.
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Spray Drying
Factors influencing stability
• Oxidation - encapsulant matrix - most important! DE effects, source variation, and Aw
• Physical - emulsion - carrier and homogenization
• Diffusional losses - carrier! Tg
• Caking - carrier (environment Aw) (silica)
23 | Reineccius G 2001 | Shen et al 2010
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Spray Drying
Factors affecting retention of volatiles
• Type of volatile
• In-feed solids
• Encapsulant material
• Homogenization
• Dryer temperatures
• Load (20% in industry - high load implications)
• Air flows (fixed by design)
0
10
20
30
40
50
60
70
80
90
ET
HY
L
AC
ET
AT
E
ET
HY
L
PR
OP
ION
AT
E
ET
HY
L
BU
TY
RA
TE
ET
HY
L
VA
LE
RA
TE
ET
HY
L
HE
XA
NO
AT
E
ET
HY
L
HE
PT
AN
OA
TE
RE
TE
NT
ION
24 | Reineccius G, 2001
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Sanguansri & Augustin | CSIRO
Spray Drying
Factors affecting retention of volatiles
• Type of volatile
• In-feed solids
• Wall material
• Homogenization
• Dryer temperatures
• Load (20% in industry - high load implications)
• Air flows (fixed by design)
CARRIER TYPE
0
20
40
60
80
30 40 50 60
INFEED SOLIDS (%)
RE
TE
NT
ION
(%
)
GUM ACACIA
N-LOK
MALTRIN M-100
DRYING TEMPS
30405060708090
70 80 90 100
EXIT AIR TEMP (C)
RE
TE
NT
ION
(%
)
INLET 247C
INLET 205C
INLET 163C
25 | Reineccius G, 2001
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Spray Drying
Factors affecting powder characteristics
• Dryer temperatures (Ti)
– Bulk density
– solubility
• Load (20% in industry - high load implications)
• Air flows (fixed by design)
26 | Fazaeli et al 2012, Food Bio Proc, 90(4): 667-675
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Prilling
Spray cooling Spray chilling Congealing
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Spray cooling / spray chilling
Sanguansri & Augustin | CSIRO 28 |
1000 kg
High melting
Fat
Warming to 90 °C
9 hours
Mixing 30 min200 kg
active
Blender
X m3 /h AirCooling to 4 °C
Heat exchanger
Reactor
Atomisation
600 kg / h
Cooling20 °c
Warming 20 °C
heat
exchange
Sieving
500 < d < 1500 µm
Cyclonic
/ Filtration
Cooling chamber
Encapsulant preparation
Core incorporation
Core Dispersion or homogenisation
Particle or Droplet
formation
Matrix or shell hardening and
stabilisation
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Spray cooling / spray chilling
Sanguansri & Augustin | CSIRO 29 |
Melt tank
Cooling chamber
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Spray cooling / Spray chilling
• Similar to spray drying but no water is evaporated and uses cold air
• Active is dispersed in a lipid melt or thermogel solution, emulsion or suspension
– spray lipid melt into cold air, allow to solidify & collect as powder
– spray thermogel solution into cold air, collect gelled particles (can be dried afterwards)
• Active on the surface can be washed with solvent
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Spray cooling / Spray chilling
Processing considerations
• Active solubility/dispersibility in lipid melt or thermogel
solution
• Melting point (is active stable)
• Solidification point (stability during handling and storage)
• Heat of crystallization / solidification
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Spray cooling / Spray chilling
• Particle size determined by:
– atomization (no shrinkage), but limited by
– time available to solidify (not dehydrate)
– air temperatures - limited by economics
– matrix viscosity (use of additives e.g. stearic acid plus ethylcellulose)
32 |
Microspheres obtained by prilling / spray chilling
(scale bar: 300 μm).
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Spray cooling / Spray chilling benefits
Application
• Examples: antioxidants, vitamins, nutritional oils, proteins, enzymes, acidulants in meat products, flavorings, leavening agents, high potency sweeteners (aspartame), yeasts, probiotics, minerals, etc
• Improve heat stability
• Delay release in wet environment
• Least expensive
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Spray cooling / Spray chilling
Factors affecting physical properties
• Melting point is critical parameter. Determined by:
- determined by fat crystalline structure
- fat/wax/polymer itself
• Influences release properties, flowability, and “caking”
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Spray cooling / Spray chilling
Factors influencing stability of active
• Encapsulant/matrix dependent
– Permeability of matrix by active - liquid/solid, solubility, etc.
– Wall thickness - uniformity
– Permeability of matrix by oxygen or moisture
– Permeability/solubility – other food components
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Coating Technologies
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Particle Coating technologies
Poncelet (2011) Microencapsulation workshop 37 | Sanguansri & Augustin | CSIRO
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Fluid bed coating
• Spray coating • spray a film forming encapsulant in hot
air
• Solidification – evaporation by drying air
• Hot melt coating
• Spray hot melt (lipid) in cold air
• Solidification - cooling to solidify the melt
• Dry powder coating /
• Spray fine powder and plasticising agent in ambient air
• Adsorption, sticking, coalescence
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Fluid bed coating application
Sanguansri & Augustin | CSIRO 39 |
Coating – layering Hot melt coating
Spraying Wetting Recrystalisation Coated Particles
Single wall multiple wall
Meiners JA, 2012, Woodhead Publishing Google images
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Fluid bed coating stabilisation
evaporat ion(drying)
coatingspray
impact, spreading,adhesion, coalescence
Cooling air
hot meltcoat ingspray
impact, spreading,adhesion, coalescence
evaporat ion(drying)
binderspray
powderspray
Drying Cooling (hot melt) Sticking / adsorption
Slow - high quality
Fast - good quality
Fast - Room temperature
40 | Sanguansri & Augustin | CSIRO Poncelet (2011)
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Example – Probiotic powder coating
Sanguansri & Augustin | CSIRO 41 |
1.E-07
1.E-06
1.E-05
1.E-04
1.E-03
1.E-02
1.E-01
1.E+00
0 1 3 5 7
Via
bil
ity
Loss
[(c
fu/g
)/(c
fu/g
)0]
Accelerated Storage (25°C x 57%RH) Time (week)
No coating
Shellac & wax coatedMicrogranule + coating
Microgranule (No coating)
Ying et al 2015, Food Aust
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0
1
2
3
4
5
6
Moi
stur
e up
take
(g
H2O
/100
g so
lids)
Time (min)
Microcapsule pellets without-coating
Microcapsule pellets with shellac-coating
H2O
BacteriaLGG
H2O
ShellacCoating
t1 t2
BacteriaLGG
Expected theoretical maximum moisture uptake of the shellac coated pellets
100 200 300 400 500
Example probiotic coating
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Spinning disk coating
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Spinning-disk coating
Sanguansri & Augustin | CSIRO 44 | Particle Coating Technologies, USA. Southwest Research Institute, USA
The solid core is suspended in a liquid encapsulant
material. The suspension is passed over a rotating disk
under controlled conditions
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Spinning-disk coating
Sanguansri & Augustin | CSIRO 45 |
• Similar to centrifugal extrusion
• the spinning disk uses rotational forces to create droplets
• Active ingredient is suspended in a wall material and dropped onto the rotating disk
• Throws the droplets out towards the circumference, the wall material solidifies through drying or chilling
• Produce matrix particles, with narrow particle size distributions between 5 and 3000 microns
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Liquid co-extrusion encapsulation
Centrifugal co-extrusion
Annular jet encapsulation
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Co-extrusion technologies
Sanguansri & Augustin | CSIRO 47 | Southwest Research Institute, USA.)
The core and shell material (two immiscible liquids) are pumped through a two fluid
nozzle. The liquid stream spontaneously breaks up into droplets
Core-shell
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Sanguansri & Augustin | CSIRO
Centrifugal Extrusion encapsulation A liquid co-extrusion process
• Nozzles consisting of concentric orifices located on the outer circumference of a rotating cylinder
• Liquid core is pumped through the inner orifice and liquid wall material through the outer orifice
• The co-extruded products breaks into droplets which forms the capsules
• The size can be as little as 150 microns
• The payload can be up to 80% by wt.
• Typical encapsulants included: gelatin, carageenan, starch, cellulose derivatives, gum arabic, fats and waxes, or polyethylene glycol.
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Annular jet encapsulation
Sanguansri & Augustin | CSIRO 49 |
A liquid co-extrusion process
• Two concentric jets, the inner (active ingredient) and the outer (molten wall material )
• Co-extruded fluid stream naturally breaks into droplets which form the microcapsule (solidifies when exiting)
• Vibrational nozzle control the droplet size down to sub-micron diameters.
• The liquid can consist of any liquids with limited viscosities e.g. solutions, emulsions, suspensions, melts etc.
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Extrusion
Carbohydrate melt extrusion High shear extrusion
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Carbohydrate (melt) extrusion encapsulation
Traditional process
1. Sugar base (plus emulsifier <2%), heated to 110 – 130°C
2. Addition of flavor or other active (8 - 10%)
3. Formation of emulsion
4. Extrusion (low shear) through die (1/64" holes) into cold isopropanol bath
5. Centrifugation – to separate capsules
6. Drying
Batch process
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Sanguansri & Augustin | CSIRO
Carbohydrate (melt) Extrusion
Melt injection process • Materials used: sucrose, maltodextrin, glucose syrup, polyols, and/or
mono- and disaccharides
• Active is mixed with molten material and pressed through one or more holes and then quenched by a cold dehydrating liquid
• The matrix material hardens on contact with the dehydrating liquid - often isopropanol and liquid nitrogen
• The size of the microcapsules is controlled by stirring – breaking up the extrudates into small pieces
• Residues of active outside the particles are washed away by the dehydrating liquid
• The microcapsules are water soluble and have particle size from 200 to 2000 microns
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Sanguansri & Augustin | CSIRO
Carbohydrate (melt) Extrusion
Factors affecting physical properties • Size - diameter largely fixed by die size, length by means
of “cutting” extrudate
• Solubility - function of matrix, size and density
• Density - generally high - result of particle forming method
• Dispersibility - rapid due to density and particle size
• Particles are generally durable
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Sanguansri & Augustin | CSIRO
Carbohydrate (melt) Extrusion
Factors influencing volatile/active retention
• Matrix composition – high sugar (caking)
• Emulsification – particle size and distribution in the matrix
• Temperatures and pressures of operation
• Volatiles incorporated - difficult to retain some volatiles (acetaldehyde, methanol, hydrogen sulfide)
• Load - usually ca. 10% although some patents claim much higher
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Carbohydrate (melt) Extrusion
Application:
• For encapsulation of volatile and unstable active (in glassy matrices)
• Has very long shelf life – gases diffuse very slowly through the glassy matrix
• Glassy matrices have good oxygen barrier properties
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Twin screw (high shear) extrusion process
Sanguansri & Augustin | CSIRO 56 |
Continuous process
• Dry feed and liquid feed added separately
• Active can be added at much later stage (shorter residence time) to minimise exposure to heat
• In the feed zone low pressure is generated to homogenise the feed
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Twin screw (high shear) extrusion process
Requirements
• Intensive mixing – even distribution of core
• Solids are melted – for improved efficiency and prevent blockage at the die
• Melt is cooled before die – to form & prevent flash-off of volatiles
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Twin screw (high shear) extrusion process
• Very similar to melt injection - uses an extruder with single or twin screw in a continuous process
• Extrudates are dry and does not go into a dehydrating liquid/solvent
• Extrudates not limited to sugars or carbohydrates as matrix
• Matrix composed of starch, maltodextrin, modified starch, sugars, cellulose, protein, emulsifiers, lipids, and/or gums
• Core is entrapped in a continuous matrix
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Summary
• The choice of microencapsulation process depends on…
– Properties of the core (liquid, solid, volatile)
– Requirements in the target food application
– Encapsulant material chosen
– Microcapsule properties (powder, size, structure, morphology)
• Develop your process taking in account commercial scale-up
• Write clear protocol that could be suitable for scale-up
• Do not forget economical aspects of your system
• It is often the COST and not the technology that hinders commercialisation
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CSIRO FOOD AND NUTRITION
Thank you Luz Sanguansri Research Team Leader
t +61 3 9731 3228 e [email protected] w www.csiro.au
Mary Ann Augustin Research Group Leader
t +61 3 9731 3486 e [email protected] w www.csiro.au