Encapsulation_LEO

Average

difference

Coefficient

βi

Significance

(%)

Conclusions

(Best
condi;ons
among
the
levels)

Encapsula;on

Efficiency
(EE)
**

Type
of

membrane

1
=
SPG;
2
=
Nylon;

3
=
Cellulose
ester

1
-‐
3
1,46
42,8
*

Not
significant
differences
among

type
of
membranes.

2
-‐
3
1,97
35,8
*

Type
of

complex

1
Complex
I;

2
=
Complex
II

1
-‐
3
-‐0,42
77,5
*

Not
significant
differences

between
complexes.

Ra;o

oil
:
wall

material

1
=
1:4;
2
=
1:3;

3
=
1:2;
4
=
1:1

1
-‐
4
6,76
1,4
1 : 4
r a O o
p r o v i d e s
h i g h e r

encapsulaOon
efficiency
than
the

others.

Maximum
=
90,36
%

Minimum
=
75,42
%

2
-‐
4
4,39
6,8
*

3
-‐
4
2,28
29,2
*

Wall
material

1
=
Maltodextrin;

2
=
Starch;

3=
Sodium
Caseinate;

4
=
Arabic
gum

1
-‐
4
-‐2,98
18,3
*

Arabic
gum
provides
a
significantly

higher
encapsulaOon
efficiency

than
starch.

2
-‐
4
-‐4,53
6,2
*

3
-‐
4
-‐1,16
57,8
*

[1]
K.
Ziani,
Y.
Fang,
D.
McClements
(2012);
Fabrica;on
and
stability
of
colloidal
delivery
systems
for
flavor
oils:
Food

Research
Intena;onal,
46,
209-‐216

[2]
J.
M.
Rodríguez,
A.
Pilosof
(2011);
Protein-‐polysaccharide
interac;ons
at
fluid
interfaces:
Food
Hydrocolloids,
25,

1925-‐1937.

[3]
A.
Tren;n,
S.
De
Lamo,
C.
Güell,
F.
López,
M.
Ferrando
(2011);
Protein-‐stabilized
emulsions
containing
beta-‐carotene

produced
by
premix
membrane
emulsifica;on,
J.
Food
Eng.
106,
267–274

[4]
V.
Paramita,
T.
Furuta,
and
H.
Yoshii
(2012);
High-‐Oil-‐Load
Encapsula;on
of
Medium-‐Chain
Triglycerides
and
d-‐

Limonene
Mixture
in
Modified
Starch
by

Spray
Drying.
J.
Food
Sci.
77,
E38-‐44.

Lemon

essen;al
oil

Spray
drying

(Water
removed)

Microcapsule

Wall
material
addi;on

Membrane

Fine
emulsion

Coarse
emulsion

Low
pressure

Mechanical
s;rring

(15000
rpm,
3
min)

!
Encapsula;on
of
lemon
essen;al
oil
using
protein-‐polysaccharide

complexes
as
emulsifiers
and
combining
oil-‐in-‐water

membrane
emulsifica;on
with
spray-‐drying

J.
Carmona,
C.
Güell*,
J.
Ferré+
and
M.
Ferrando

Departament
d’Enginyeria
Química

+
Departament
de
Química
AnalíOca
i
Química
Orgànica,

Universitat
Rovira
i
Virgili,
Spain
Avda.
Països
Catalans,
26,
43007
Tarragona
(Spain)

Tel:
+34977558504;
email:
carme.guell@urv.cat

Protein-‐polysaccharide
complexes
as
emulsifiers

Materials
&
Methods

Introduc;on
&
Aim

Flavour
is
one
of
the
most
important
characterisOcs
of
a
food
product.
The
need
for
food
products

that
are
tasty,
healthy
and
convenient
will
conOnue
to
demand
improved
aroma
delivery
systems,

which
might
be
achieved
by
modifying
the
exisOng
encapsulaOon
processes
or
by
combining
the
exisOng

ones
[1].

The
aim
of
this
study
was
to
produce
microcapsules
of
lemon
essenOal
oil
using

complexes
replacing
convenOonal
emulsifiers
[2]
with
Premix
membrane
emulsificaOon
(ME)
[3]
to

obtain
oil-‐in-‐water
(O/W)
emulsions
and,
subsequently,
applying
spray-‐drying
[4].
An
Asymmetric

Screening
Design
was
used
to
idenOfy
the
operaOng
condiOons
having
a
major
impact
on
the

encapsulaOon
efficiency
(for
example,
wall
material
or
type
of
complex).

Membrane

Emulsifica;on

(Three
cycles)

Experimental
design

Conclusions

The
authors
acknowledge
funding
from
the
Spanish
Ministry
of
Economy
and
Compe;;veness
for
suppor;ng
this
research
work
(Project

funding
CTQ2011-‐22793
and
AGL2011-‐264566)
and
Dallant
S.A
for
providing
the
essen;al
oil
and
technical
support.
Jaume
Carmona
thanks

Universitat
Rovira
i
Virgili
for
his
scholarship.

Factor 1 Factor 2 Factor 3 Factor 4
Type
of membrane
Wall material
Ratio
Lemon oil : Wall material
Type
of complex
SPG
MD
(ME
-‐
20)
1:4

Complex
1

Nylon
Midó
1:3

Cellulose
ester
NaCAS
1:2

SPG
Arabic
gum
1:1

SPG
Midó
1:2

Complex
2

Nylon
MD
(ME
-‐
20)
1:1

Cellulose
ester
Arabic
gum
1:4

SPG
NaCAS
1:3

SPG
NaCAS
1:1

Complex
1

Nylon
Arabic
gum
1:2

Cellulose
ester
MD
(ME
-‐
20)
1:3

SPG
Midó
1:4

SPG
Arabic
gum
1:3

Complex
2

Nylon
NaCAS
1:4

Cellulose
ester
Midó
1:1

SPG
MD
(ME
-‐
20)
1:2

Fluxes
during
Premix
membrane
emulsifica;on

References

Premix
ME
in
combinaOon
with
spray-‐drying
enable
to
successfully
encapsulate
lemon
essenOal
oil
when
WPI-‐polysaccharide

complexes

were
used
as
emulsifiers.

The
results
from
the
asymmetric
screening
design
showed
that
only
the
type
of
membrane
had
a
significant
impact
on
the

emulsion
droplet
size.

Regarding
encapsulaOon
efficiency,
both
wall
material
and
oil
to
wall
material
raOo
exhibited
a
significant
effect.

Results

Droplet
size
(D3,2)
during
Premix
membrane
emulsifica;on

Cellulose
ester

Figure
3.

ESEM
images
of
external
and
internal
morphology
of
lemon
oil
microcapsules:
a)
Complex
I,
raOo
1:1,
NaCAS
and
glass
membrane;
b)
Complex
II,
raOo
1:1,

starch
and
cellulose
ester
membrane.

Figure
1.

Emulsion
flux
for
each
emulsificaOon
cycle
using
Nylon
(a)
and
Cellulose
ester
membrane
(b)
with
different
complexes.

Membrane
Porous
size
(μm)
Membrane
configuration
Diameter/ length
(mm)
Type
of membrane
Wettability
Working
pressure
(MPa)
Nylon 0,8
Flat
47
Organic
Hydrophillic
0,7

Cellulose
ester
0,8
Flat
47
Organic
Hydrophillic
0,7

SPG* 1,0
Tubular
100
Inorganic
Hydrophillic
0,2

Experimental
condi;ons
during
Premix
ME

Model:
Asymmetric
Screening
Design

Responses
of
interest:
droplet
size
(D3,2)
at
the
end
of
Premix
ME
and
oil
encapsulaOon
efficiency
(EE)

Number
of
experiments:
16
plus
4
replicates

Number
of
factors:
4

Factor
levels:
Factor
1:
3
levels;
Factor
2:
4
levels;
Factor
3:
4
levels;
Factor
4:
2
levels

This
model
enables
to
idenOfy
the
factors
having
a
major
impact
on
the
responses
using
equaOon
1.

Xvx

Eq.
1

Y
=
b0
+
b11
·∙
x11
+
b12
·∙
x12

+
b13
·∙
x13

+
…
+
bn
·∙
xn

Where
Y
is
the
predicted
response;
b0
is
the
intercept
term;
bn
is
the
linear
coefficients;
xn
is
the
average

values
for
each
factor
fixed.

Experiments

Figure
2.

Progress
of
mean
droplet
size
during
Premix
membrane
emulsificaOon
using
Nylon,
Cellulose
ester
and
SPG
membranes

with
Complex
I
(a)
and
Complex
II
(b).
Droplet
size
of
the
coarse
emulsion
corresponds
to
Cycle
0.

(a)
(b)

Results
of
the
Asymmetric
Screening
Design

External
and
internal
morphology
of
lemon
oil
microcapsules

Acknowledgment

(b)
(a)

Response
Factor
Levels

Average

difference

Coefficient

bn

Significance

(%)

Conclusions

Droplet
size
(D3,2)
of

the
end
of
Premix
ME

Type

of
membrane

1
=
SPG;

2
=
Nylon;

3
=
Cellulose
ester

1
-‐
3
-‐0,13
87,0
*

Only
significant
differences

between
Nylon
and
Cellulose
ester

membranes.

Nylon
membranes
produces

smaller
droplets.

2
-‐
3
-‐2,21
4,02

Type

of
complex

1
=
Complex
I;

2
=
Complex
II

1
-‐
3
0,75
25,6
*

Not
significant
differences
between

complexes.

*
Significance
values
above
than
5%
are
not
significant.

**
The
encapsulaOon
efficiency
(EE)
was
calculated
with
this
equaOon:

Eq.
2

EE
=
((TO
-‐
SO)
/
TO)
·∙
100

Where
TO
is
the
total
amount
of
lemon
essenOal
oil
in
the
microcapsule
and
SO
on
the
surface.

Protein
Polysaccharide

pH
=
7.0

Acidifica;on

pH
=
3.8

Oil
phase
Water
phase

Interphase

Complex

forma;on

Complex Protein (wt/wt %) Polysaccharide (wt/wt %)
I Whey
Protein
Isolate*
(0,5
%)
Carboxymethyl
Cellulose
(0,25
%)

II Whey
Protein
Isolate*
(0,5%)
Arabic
gum
(0,5
%)

Produc;on
of
lemon
essen;al
oil
microcapsules

0,0

0,5

1,0

1,5

2,0

2,5

3,0

3,5

4,0

1
2
3

Flux
(Kg/m2·∙s)

Premix
ME
Cycle

Complex
I

20%
oil
+
Nylon

20%
oil
+
Metricel

0,0

0,5

1,0

1,5

2,0

2,5

3,0

3,5

4,0

1
2
3

Flux
(Kg/m2·∙s)

Premix
ME
Cycle

Complex
II

20%
oil
+
Nylon

20%
+
Metricel

0

2

4

6

8

10

12

14

0
1
2
3

D
3,2

Premix
ME
Cycle

Complex
I

20%
oil
+
Nylon

20%
oil
+
Metricel

20%
+
SPG

0

2

4

6

8

10

12

14

0
1
2
3

D
3,2

Premix
ME
Cycle

Complex
II

20%
oil
+
Nylon

20%
oil
+
Metricel

20%
oil
+
SPG

Cellulose
ester

Water

+

Complex

Inlet
Temperature
=
170
oC

Outlet
Temperature
=
60
oC

Pump
rate
=
6
mL/
min

Air
flow
rate
=
35
m3/
h

Cellulose
ester

Cellulose
ester

*
Shirasu
porous-‐glass.

Table
1.

Levels
for
each
factor
as
a
result
of
the
asymmetric
screening
design
model.

b
a

*
WPI.

oil
+
Cellulose
ester

oil
+
SPG

a

Encapsulation_LEO

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