ZENIA ADIWIJAYA

COORDINATION WITH: EVANDRO

MARTINS

CAPSULES PRODUCED WITH W/O AND O/W EMULSIONS

INVERSE GELATION MECHANISM

• ABANG et al. (2012)

O/W emulsion (27.7 g/L of CaCl2)

• ANDERSON (2010)

W/O emulsion (176 g/L of CaCl2)

W/O Emulsion destabilizers

RELEASE OF Ca2+ FROM THE EMULSIONS

Oil CaCl2 Solution Membrane

O/W EMULSION W/O EMULSION

3

Ca

Ca

Ca

CaCa

Ca

CaCa

Alginate Solution

Ca Ca

Ca

Ca

Ca

Ca

Ca

Ca

Ca

CaCa

Ca

Ca

Ca

Ca

CaCa

Ca

Ca

Ca

OBJECTIVES

4

• To optimize the production of capsules using W/O emulsion

by reducing CaCl2 concentration

• To compare capsules produced with W/O and O/W emulsions

5

Capsules

EXPERIMENTS

W/O EMULSION

6

100 mL Oil +

30 mL CaCl2

solution(240 g/L)

+SPAN 85 or PGPR

90

W/O EMULSIONS FORMULATIONS

W/O EMULSIONS FORMULATIONS

7

Concentration (g/L)

SPAN 85 PGPR 90Size of water droplets (μm) Stability Size of water

droplets (μm) Stability

0.08 19 ± 7 15 min 15 ± 6 50 min

0.8 14 ± 5 18 min 7 ± 1 1 day

8 14 ± 8 20 min 0.7 ± 0.1 5 day

SPAN 85

PGPR 90

8

CAPSULES PRODCUTION: W/O EMULSION

W/O EMULSION

CaCl2 : 4.6 - 55.4

g/L

EMULSION

DESTABILIZERS

TWEEN 20

ETHANOL OR

ACETONE

9

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

Ethanol Acetone

Mem

bran

e th

ickn

ess

(mm

)

Series10

5

10

15

20

25

30

35

40

45

Ethanol Acetone

% M

Ethanol Acetone

EFFECT OF DESTABILIZERS: ETHANOL/ACETONE

Acetone is the best

destabilizer

AW ALGINATE SOLUTIONS

10

Alg Alg +T20/Ethanol Alg +T20/10% acetone Alg+T20/20% acetone0.982

0.984

0.986

0.988

0.99

0.992

0.994

0.996

0.998

AW

AW π

MECHANISM OF DESTABILIZATION: ACETONE

11

ACETONE

Ca

CaCa

Ca

CaCa

Ca

12

0 10 20 30 40 50 600

0.51

1.52

2.53

3.54

4.55

CaCl2 Concentration (g/L)

Dia

met

er (m

m)

0 10 20 30 40 50 600

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

CaCl2 Concentration (g/L)

Mem

bran

e th

ickn

ess

(mm

)

0 10 20 30 40 50 600

10

20

30

40

50

60

70

CaCl2 Concentration (g/L)

%M

EFFECT OF CaCl2 CONCENTRATION

Minimal CaCl2 concentration:

13.8 g/L

13

Capsules

EXPERIMENTS

O/W EMULSION

100 mL Oil +

30 mL solution CaCl2

+0.5 mL Span 85/

Tween 85

14

CAPSULES PRODCUTION: O/W EMULSION

O/W Emulsion Production Capsules Production

15

EFFECT OF CaCl2 AND ALGINATE CONCENTRATIONS

55.4 27.713.84.6

CaCl2 Concentration (g/L)15

10

5

Algi

nate

Con

cent

ratio

n (g

/L)

16

0 10 20 30 40 50 600

0.51

1.52

2.53

3.54

4.55

CaCl2 Concentration (g/L)

Diam

eter

(mm

)

0 10 20 30 40 50 600

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

CaCl2 Concentration (g/L)

Mem

bran

e th

ickn

ess

(mm

)

0 10 20 30 40 50 600

10

20

30

40

50

60

70

CaCl2 Concentration (g/L)

% M

EFFECT OF CaCl2 AND ALGIANTE CONCENTRATIONS

• Alginate 5 g/L

• Alginate 10 g/L

• Alginate 15 g/L

17

Capsules

EXPERIMENTS

O/W AND W/O EMULSION

18

CAPSULES: W/O AND O/W EMULSION

55.4 27.713.8

CaCl2 Concentration (g/L)O

/WW

/O

Algi

nate

10

g/L

19

6.9 13.8 27.7 55.40

5

10

15

20

25Dry Capsules

CaCl2 concentration (g/L)

Rupt

ure

Forc

e (N

)RUPTURE FORCE: W/O AND O/W EMULSION

• W/O

• O/W

RF = 0.4 (Ca) -1.8

RF = 0.2 (Ca) + 22

LOG(MEMBRANE VOLUME) (Vm) X LOG (CORE VOLUME) (Vc)

20

Vm= K Vc

Vm =6 10-2 Vc4 - 24 Vc3 + 130 Vc2 – 249

Vm= 0.1 Vc4 + 5 Vc3 -63 Vc2 +351 Vc - 718

• THEORICAL CURVE

• W/O EMULSION

• O/W EMULSION

Vm

Vc (μm3)

CAPSULESMICROCAPSULES

21

% MEMBRANE (%M) x LOG (CORE VOLUME) (Vc)%

M

Vc (μm3)

%M = K/K+1

%M =6 10-3 Vc5 - 0,3 Vc4 + 5 Vc3 – 43 Vc2 + 185 Vc - 315

%M = 5 10-3 Vc5 - 0,2 Vc4 +4 Vc3 – 34 Vc2 + 143 Vc - 229

CAPSULESMICROCAPSULES

• THEORICAL CURVE

• W/O EMULSION

• O/W EMULSION

22

• Easier to get

• Do not need additional destabilizer

• More uniform/ homogeneous in shape

• Membrane slightly weaker

• Minimal concentration of CaCl2: 4.6

g/L

• Harder to get

• Need additional destabilizer

• Lower CaCl2 released

• More heterogeneous in shape

• Membrane slight stronger

• Minimal concentration of CaCl2: 13.8 g/L

O/W W/O

CAPSULES: W/O AND O/W EMULSION

CONCLUSION

23

• Capsules using W/O emulsions with less CaCl2 can be obtained

• The properties of the capsules produced with W/O and O/W are similar

• The release of Calcium ions from the emulsion depends on the core

size and the emulsion

• Capsules produced with W/O emulsions cannot be used in food areas

due to the utilization of acetone

MERCI!