1.
WELCOME
1

2.
Dept.PMA
UNIVERSITY OF AGRICULTURALAND HORTICULTURAL
SCIENCES –SHIV
AMOGGA
COLLEGE OF HORTICULTURE, MUDIGERE
Name of the Student
I.D.No.
Degree Programme
Department
:Tamanna Arif
:MH2TAI240
: Sr. M.Sc. (Hort.)
: PSMAC
Seminar - I
on
Microencapsulation in spices
2

3.
11/01/2020 Dept. PMA
4
 What is microencapsulation?
 History
 Application of microencapsulation
 Need for encapsulation in spices
 Morphology of microcapsules
 Methods of encapsulation
 Case studies
 Conclusion
TOPIC DIVISION
3

4.
What is microencapsulation?
• Microencapsulation is defined as a process in
which tiny particles or droplets are surrounded by
a coating or embedded in a homogeneous or
heterogeneous matrix, to give small capsules.
• Size range :1 to 1000 μm in diameter
11/01/2020 Dept. PSMAC (Poshadri and Aparna, 2010) 4

5.
HISTORY
)
 In 1932, introduction of microencapsulation procedure by
Bungen burg de John
 Origin of microencapsulation lies in paper industries by 1940s
 Commercial product - microencapsulated ink by
America in 1953 (Complex coacervation)
 Textile industry started introducing many encapsulated products in
between 1960 and 1970
 Pharmaceutical industry has long used microencapsulation for
capsule preparation.
 Late 1970’s exploration in agriculture, food, cosmetic industries
5

6.
• The material to be coated is
called core material
• Core materials are either
solids, liquids or a mixture
of these such as dispersion
of solids in liquids.
• Core material proportion:
20-95% w/w
(Bansode et al., 2010)
• It is a shell or covering
material which protect core
material from deterioration
and evaporation of
volatiles.
• Example: Gums, lipids,
proteins, carbohydrates,
celluloses etc
• 0.5-150µm thick
(Snehal et al., 2013)
11/01/2020 Dept.PMA
CORE MATERIAL WALLMATERIAL
6

7.
Characteristics of wall material
• Stabilization of core material.
• Chemically compatible and non reactive.
• Pliable, stable and non- hygroscopic.
• Low viscosity.
• Soluble in an aqueous media or solvent.
• Inexpensive, food-grade status.
• Should be flexible, hard, thin, impermeable .
Dept.PSMAC ( Saikiran et al., 2018) 7

8.
Commonly used coating materials in food industry
Dept.PSMAC
Natural polymers Synthetic polymers
• Proteins:
Albumin
Gelatin
Collagen
• Carbohydrates:
Chitosan
Starch
Poly dextran
Poly starch
• Gums
Gum arabic
Sodium alginate
• Lactides
• Glycolides
• Poly alkyl cyano acrylates
• Poly anhydrides
(Suganya et al., 2017) 8

9.
Application of microencapsulation
Agriculture
Animal nutrition
(Dubey et al., 2009)
9

10.
Dept.PMA
• Spice oleoresin- complete flavor profile of spices
• Highly concentrated and viscous
• Usually volatile and chemically unstable
• Poor storage life
• Immiscible in aqueous matrix
(Dubey et al., 2009)
Why in spices ??
10

11.
• Conversion of liquids to free flowing solids
• Lowers volatility and increases shelf –life of fragrance
• Masking of odour, taste and activity of encapsulated
materials
• Provide protection from environment and oxidation
• Controlled release of active compounds
• Improves bioavailability and stability
Need for encapsulation
(Dubey et al., 2009) 11

12.
Methods of encapsulation
• Spray- drying
• Spray chilling
• Extrusion
• Fluidized bed coating
• Lyophilization
• Coacervation
• Co-crystallization
• Inclusion complexation
12

13.
2. Spray chilling
Dept.PSMAC
( Saikiran et al., 2018) 13
Particle size: 20- 200 µm

14.
3. Extrusion
• Encapsulation of volatile and unstable flavours in glassy
carbohydrate matrices.
• Microcapsules have very long shelf life.
• Commercially used for encapsulating nutraceuticals.
11/01/2020 Dept.PMA
(Quellet et al., 2001)
0.25-2mm
(0–500 atm and 70–500°C)
14

15.
4. Fluidized bed coating
• Also known as suspension coating
• Principle : Spraying - Evaporation
• Coating materials used are melted fats, waxes or
emulsifiers as shell materials.
• Particle size: 20 to 1000μm
0 Dept.PMA
( Saikiran et al., 2018)
15

16.
5. Lyophilization
Dept.PSMAC
• Dehydration of heat sensitive materials and aromas.
• Sample frozen (-90 to -40oC)
• Particle Size – 20µm to 5mm
(Shami and Bhasker, 2009)
16

17.
6. Coacervation
• Known as Phase separation method
• Core material is dispersed in the solution of coating material.
The shell starts to precipitate from the solution.
• Commonly used wall material- Gum arabic and gelatin.
• Particle size: 10–800µm
Dept.PSMAC
(Nicolaas and Shimoni , 2010)
17

18.
Schematic representation of coacervation
Dept.PSMAC
(Nicolaas and Shimoni , 2010)
Contd..
18

19.
7. Co-crystallization
Dept.PSMAC
• New encapsulation process
• Wall material – Sucrose
Flow-chart of co-crystallization process
Sucrose syrup
(supersaturated state )
Addition of
core material
Vigorous
Mechanical
agitation
Nucleation
Crystallize
Agitation is continued Agglomerates are discharged Dried
(Sanjoy Kumar Das et al., 2011) 19

20.
8. Inclusion complexation
• Achieving encapsulation - molecular level
• Encapsulating medium - β-cyclodextrin
• Guest molecules – entrapped (dimensionally) by
hydrophobic interaction.
• Internal cavity - 0.65nm diameter
• Particle size - 0.001– 0. 01µm
Dept.PSMAC (Poshadri and Aparna, 2010) 20

21.
Dept.PMA
Diffusion
Temperature
sensitive
Solvent- activated
Pressure activated
Swelling
pH -controlled
Controlled
release
mechanism
(Jeyakumari et al.,2016)
21

22.
11/01/2020 5
22

23.
Type Oleoresin
t1/2
(weeks)
Gum arabic
t1/2
(weeks)
Modified starch
t1/2
(weeks)
EP - -
Y=‒0.0097x +4.601
R²= 0.921
71.44
Y= ‒0.0126x + 4.601
R² = 0.959
55
TP
Y= ‒0.125x + 4.604
R² = 0.994 55.44
Y= ‒0.0057x + 4.604
R² = 0.943 121.57
Y= ‒0.0054x +4.603
R² = 0.958 120.33
TV
Y= ‒0.0295x +4.606
R² = 0.999 23.49
Y= ‒0.0269x +4.605
R² = 0.997 25.76
Y= ‒0.0263Xx+ 4.618
R² = 0.972 26.34
NV
Y= 0.0098x + 4.6045
R² = 0.999 70.71
Y= 0.0089x+ 4.6007
R² = 0.981 77.86
Y= 0.0167x+ 4.5969
R² = 0.981 41.49
Dept.PSMAC
Table 1. Analysis for *EP, TP, TV and NV in free and encapsulated oleoresin
Oleoresin at 2.5 % based on carrier materialused
R2 indicated correlationcoefficient
(Shaikh et al., 2006)
*EP- Entrapped piperine
TP- Total piperine
TV- Total volatiles
NV- Non-volatiles
23

24.
Dept.PSMAC
(b) Modified starch HiCap-100
Size: 7-20 µm
Nearly spherical with smooth surface
Size: 5-15 µm
Nearly spherical with smooth surface
(Shaikh et al., 2006) 24
Fig. 1. Scanning electron microscopic image of spray
dried microcapsules
(a) Gum arabic

25.
Dept.PSMAC
(Xiao et al., 2014)
MEY- Microencapsulation Yield
MEE- Microencapsulation Efficiency
25
Fig. 2. Effect of emulsification temperature on the morphology,
efficiency and yield of capsanthin microcapsules

26.
Dept.PSMAC
Fig. 3. Effect of wall concentration on the morphology,
efficiency and yield of capsanthin microcapsules
(Xiao et al., 2014)
MEY- Microencapsulation Yield
MEE- Microencapsulation Efficiency
26

27.
Dept.PSMAC
Fig. 4. Effect of core to wall ratio on the morphology,
efficiency and yield of capsanthin microcapsules
(Xiao et al., 2014)
MEY- Microencapsulation Yield
MEE- Microencapsulation Efficiency
27

28.
Fig. 4 Effect of temperature on
the stability of capsanthin in
microcapsules
Fig. 5.Stability of capsanthin in microcapsule in dark (a) and outdoor light (b)
(Xiao et al., 2014)
(a) Dark (b) Outdoorlight
28

29.
• Optimum conditions for capsanthin microencapsulation -
emulsification temperature 45°C, wall concentration 15 g/l and
core to wall ratio 1:2 (w/w)
• Under these conditions, droplets in emulsion were even in
size distribution without agglomeration.
• Microencapsulation increased the stability of capsanthin
against heat and light.
Dept.PSMAC
Xiao et al., 2014 29

30.
Dept.PMA
(Balasubramani et al., 2015)
30
Fig. 6. Effect of process parameters on encapsulationefficiency of garlic

31.
Dept.PSMAC
Fig. 7. Determination of optimum
conditions
Fig. 8. Scanning electron
microscopic image of
microcapsules
(Balasubramani et al., 2015)
31

32.
EE(%) CR(%) Watercontent(
% dry basis)
Solubility(%)
MD:GA(75:25) 11.78 ± 0.51g 40.35 ± 1.01h 4.81 ± 0.06a 91.69 ± 0.04d
MD:GA(50:50) 24.60 ± 0.49e 49.59 ± 0.00f 2.14 ± 0.04de 96.50 ± 0.05ab
MD:GA(25:75) 40.56 ± 0.05b 65.46 ± 0.13b 2.40 ± 0.08d 95.65 ± 0.25bc
GA (100) 16.73 ± 0.19f 24.87 ± 0.18k 4.12 ± 0.05b 92.57 ± 0.28cd
GA:MS(25:75) 32.74 ± 0.15d 68.43 ± 0.44a 1.58 ± 005f 99.25 ± 0.00a
GA:MS(50:50) 45.23 ± 0.04a 59.15 ± 0.19d 2.14 ± 0.05de 95.63 ± 0.53bc
MS (100) 11.84 ± 1.70g 55.48 ± 0.17e 1.01 ± 0.06gh 96.80 ± 0.45ab
MD:MS(75:25) 20.72 ± 0.35f 31.33 ± 0.00j 2.90 ± 0.00c 97.35 ± 0.15ab
MD:MS(50:50) 7.96 ± 0.38h 35.41 ± 0.00i 1.30 ± 0.01fg 97.88 ± 0.83ab
MD:MS(25:75) 18.94 ± 1.32f 41.61 ± 0.36h 0.84 ± 0.16h 95.90 ± 0.02abc
MD (100) 36.37 ± 1.36c 36.02 ± 0.74i 2.98 ± 0.03c 97.75 ± 0.45ab
MD:GA:MS(17:66:17) 31.51 ± 0.03d 36.35 ± 0.32i 2.78 ± 0.68c 96.90 ± 0.02ab
MD:GA:MS(33:33:33) 33.84 ± 0.39d 45.21 ± 0.39g 2.35 ± 0.24de 97.33 ± 0.07ab
MD:GA:MS(66:17:17) 33.18 ± 0.29d 54.82 ± 0.08e 2.78 ± 0.44c 85.35 ± 0.50e
MD:GA:MS(17:17:66) 31.23 ± 0.60d 61.98 ± 0.35cd 2.10 ± 0.09de 86.83 ± 0.48e
Table 2: Properties of turmeric oleoresin microcapsules produced with different
wall material formulations. (Canohiguita et al., 2015)
32

33.
Dept.PSMAC
Fig. 9. Response surface and contour
plots for Moisture content
Fig 10. Response surface and contour
plots for Particle size
( Noshad et al., 2015)
33

34.
Dept.PSMAC
Fig. 12. Morphology of microcapsules
at optimal model point
(184°C, 8.5%. 0.36%)
Fig .11. Response surface and contourplots
for Encapsulation efficiency
(Noshad et al., 2015)
34

35.
• Optimal condition for vanillin microencapsulation
found in 184ºC with 8.5 per cent malto dextrin
concentration and 0.36 per cent vanillin
concentration to obtain maximum encapsulation
efficiency (58.3%) and minimum moisture content
(3.153g/100g) and particle size (6.95µ)
Dept.PSMAC
(Noshad et al., 2015)
35

36.
Table. 3. Overview of microencapsulation in various spices
Encapsulated
material
Wall material Method Remarks
Cardamom oleoresin
(Savitha, 2005)
Gum arabic,
Maltodextrin,
modified starch
Spray- drying
Gum arabic was found to be
better wall material than
maltodextrins and modified
starch
Turmeric oleoresin
(Kshirsagar et al., 2008)
Gum arabic
and maltodextrin
Spray - drying
Gum Arabic supplemented with
1% pullulan proved to be a
better wall material in terms of
stability and film forming ability
for encapsulation of turmeric
oleoresin
Ethyl vanillin (Verica et
al., 2008)
Alginate gel Extrusion
Release of ethyl vanillin occurs
at about 260°C
Dept.PSMAC (Renu and Zehra, 2015)
36

37.
Encapsulated
material
Wall material Method Remarks
Ginger oleoresin
(Kadam et al.,2010)
Acacia gum Spray- drying
Inlet temperature of 160°C was
optimum in encapsulating
ginger oleoresin
Star –anise oleoresin
( Wang et al., 2011)
Maltodextrin and
soy protein
Spray- drying
Encapsulate of 5% oleoresin
with 20% maltodextrin and 7.5%
soy protein at an inlet
temperature of 180°C was
considered as best
Nutmeg oleoresin
(Arshad et al., 2014)
Gum arabic, Native
and modified
sorghum starches
Spray- drying
The highest oil retention of 95%
with 84.07% encapsulation
efficiency was achieved when
GA: NA starch was used in the
fraction of 25:75.
Dept.PSMAC
Contd..
(Renu and Zehra, 2015)
37

38.
Dept.PSMAC
38

39.
S.No. Encapsulated oleoresin Price (Rs/kg)
1. Black pepper 1850
2. Cardamom 7000
3. Turmeric 2500
4. Ginger 1350
5. Garlic 1000
6. Nutmeg 1200
Dept.PSMAC https://www.synthite.com 39

40.
CHALLENGES
•To produce effective encapsulated products,
the appropriate selection of coating material
is a great challenge.
•Multidisciplinary based research approach
and consideration of industrial requirements
and constraints has to be carried out.
40

41.
Conclusion
Dept.PSMAC 41

42.
11/01/2020 Dept.PMA 53
42