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J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone +34 94 601 25 [email protected] 5 th Euro-Global Summit and Expo on Food & Beverages June 16 – 18, Alicante, Spain QUALITY VALORIZATION OF MICROENCAPSULATED PROBIOTICS DEHYDRATED BY MICROWAVE DRYING

J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

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Page 1: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

J.I. Lombraña

Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. *P.O Box 644. 48080 Bilbao (Spain). Phone +34 94 601 25

[email protected]

5th Euro-Global Summit and Expo on

Food & Beverages June 16 – 18, Alicante, Spain

QUALITY VALORIZATION OF MICROENCAPSULATED

PROBIOTICS DEHYDRATED BY MICROWAVE DRYING

Page 2: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Research GroupB

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Page 3: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Functional foods

FF or nutraceuticalsaid specific bodily functions

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Probiotics

Page 4: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Functional food

• The term functional foods was first introduced in Japan in the mid-1980s and refers to processed foods containing ingredients that aid specific bodily functions in addition to being nutritious.

• In this way, a nutritionally more complete product is obtained, by adding, probiotics, vitamins and proteins, in most cases.

• There has been a rising interest in producing probiotics, the most frequent FF because of their transcendence on health beneficial effects.

• FF and specially probiotics are specially sensible material that requires protection.

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Page 5: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Probiotics

Inmunomodulation

Metabolic effects

Normalised microbiota composition

lactobacillus acidophilusbeneficial strain (DDS-1)

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Page 6: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Encapsulation

• The encapsulation searches to protect the nutritional extra added value during drying and cocking process which suffers the food.

• Capsules are formed mixing the added components with support materials (gelatine, alginate, sugars…) forming spherical particles depending on the technique used.

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Page 7: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Microencapsulation Techniques

… probiotics

Extrusion techniqueEmulsion techniqueRennet-gelled protein encapsulation

Combination of encapsulation and drying

Freeze dryingSpray DryingFluid bed

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Page 8: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Extrusion TechniqueB

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Page 9: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Probiotic elaboration

Mixing(homogenization)

Micro-encapsulation

Jet-cutting+

(droplet jelling)

Drying

Alginate sol.

+Cell culture

Fix-fluidized bed+

Microwaves

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Page 10: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Conventional Drying

The conventional drying process (convective heating), dries the product from out to inside, so the energy is applied from the surface of the product.

There is a significant loss of energy for heating the surroundings where drying occurs.

The high thermal level in conventional drying is the cause of low efficiency in the process and thermal damage.

General drawback - longer drying period and higher drying temperature for sensible products.

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Page 11: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Microwave Drying

In microwave heating, the heat is generated inside the product, favoring heat distribution due to agitation of the polar molecules contained in it.

the inverse temperature gradient, favors the drying of the particles from inside out.

Microwave drying utilizes very fast volumetric heating reducing temperature and operating times.

MW drying offers to shorten the drying time without degradation of final quality of the dried product

Page 12: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Fix-fluidized bed

Fix-fluidized bed and MW heating are specially indicated for drying: fix-fluidized microwave drying (FFMWD).

During the packed bed periods : Allows Better heat distribution by conduction

inter-particles. avoids superheated spots with enough

circulating air.

During the fluidized bed periods: Fluidized bed is used to homogenize and

control temperature. Fluidization favours mass transfer.

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Page 13: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Objectives

The main objective of the our research is to find the optimum operating conditions for FFMWD

Analysis of Drying kinetics.• Drying parameter estimation through fitting

experimental data to the mathematical model.• Moisture content and • Drying rate profiles for each thermal level

applied

Quality of dehydrated product.• Water activity profiles• Results of final water content (KF %)• Post drying cell viability

Selection of the most suitable drying condition under quality and kinetic criteria.

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Page 14: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Methodology

• Suspension preparationo 3% Sodium alginateo 10% of a cell suspension of

Saccharomyces cerevisiae ,

• Microencapsulation Technique: Jet Cutting. p 0,225 cm.

• Drop in 2% Calcium cloride solution.

Encapsulated Probiotic material

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Page 15: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Equipment

Control VariablesF: Inlet air flowTin:Inlet air TemperatureTf: Control product

temperature (MW Power)

FTin

Tf

(1)Dehumidifier , (2) Heater-cooling,(3) Microwave chamber,

(4)Temperature Display

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Page 16: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Drying experiments monitoring

Measuring control variables.• F: Inlet air flow . Vair 1.7 to 1 m/s • Tin: Inlet air Temperature• Tf: Control product temperature (MW Power)

Mass loss along drying. Build-in scale.

Moisture content• water activity (aw) along the process.• Water content. Karl Fischer

Cell viability after drying. • Units forming colony (ufc/d.s.)

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Page 17: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Control Variables

Air velocity

Air Temperature

P. surfaceTemperatureTs* / Ts

ExternalT. Gradient

P. surface temperature Ts*Controlled by the MW power Measured through Tf film or inter-particle temperature. Levels:

L 15ºCM 35 ºCH 55ºC

Air temperature Tin

Controlled by the heating device at the entrance

External gradient: Ts*- Tin. Levels: L 15ºC

M 30ºCH 50ºC

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Page 18: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Experiments planification

Phase I Phase II Phase IIICode

Exp. Tin Tf TS* Tin Tf TS

*

Decre.Temp.

1 5 20 35 5 20 35 MM/MM

2 5 20 35 20 27.5 35 MM/ML

3 5 30 55 40 47.5 55 HH/HL

4 20 27.5 35 5 20 35 ML/MM

5 20 27.5 35 20 27.5 35 ML/ML

6 20 37.5 55 40 47.5 55 HM/HL

7 20 37.5 55 20 27.5 35 HM/ML

8 40 47.5 55 40 47.5 55 HL/HL

9 40 47.5 55 20 37.5 55 HL/HM

Air flowPhase I: 5 Nm3/h (1.7 m/s) Phase II: 3 Nm3/h (1 m/s)

Letter T (ºC)

M 35

H 55

1st letter Thermal level Ts

*Letter T (ºC)

L 15

M 30

H 50

Second letter Gradient

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Page 19: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Drying selection

Best dryin

g strate

gy

Water activity

(aw)

Drying kinetics

Cell viabilit

y

Energy valorisat

ion

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Page 20: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Drying Kinetics

0 20 40 60 80 1000

1

2

3

4

5

6

Modelled

time (min)

M (

g H

2O

/g d

.s)

0 20 40 60 80 1000

0.04

0.08

0.12

0.16

time(min)

-dM

/dt

0 20 40 60 80 1000

1

2

3

4

5

6Modelled

time (min)

M (

g H

2O

/g s

s)0 20 40 60 80 100

0.00

0.10

0.20

0.30

time (min)

-dM

/dt

Exp 1

Exp 1

Exp 9

Exp 9

Phase I

Ph

ase

II Phase III

Phase I Phase IIIPh

ase

II

Ph

ase

I

Ph

ase

II

Phase III

Phase III

Ph

ase

I

Ph

ase

II

Exp 1. Excessive low temperature (Exp1-Tin=5ºC ) can cause cell damage so as the high temperature (Exp9-Tin=55ºC). Extreme drying kinetics are unfavourable

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Page 21: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Water activity

01234560

0.2

0.4

0.6

0.8

1

Exp.2

Exp.9

M [g H2O/g ss]

aw

Phase I Phase II

Phas

e II

I

0 50 100 150 200 250 3000

0.2

0.4

0.6

0.8

1

Exp.2

Exp.9

time (min)

aw

Phase III is decisive for the cell viability. A fast lowering of aw of Exp 2 is recommended

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Page 22: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Energy efficiency

0 10 20 30 40 50 600

10

20

30

40

Ts

Tair

Tf

t(min)

T(º

C)

CodePhase I Phase II

Taire Tf Ts* Taire Tf Ts

*

HH/HL 5 30 55 40 47,5 55

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In the experiment 3 (HH/HL)Convective losses are low. Onlyin Phase I, Ts>Tair

Page 23: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Quality and kinetic valorization

Exp. rI-II Mfin II rglobal

time (min)

(%)KFfin

Viablility (%)

Code

10,11

40,783 0,017 275 6,726 0,0 MM/MM

20,12

60,946 0,024 184 7,522 96.3 MM/ML

30,21

91,245 0,021 231 7,706 93.9 HH/HL

40,18

40,945 0,023 240 7,577 88.6 ML/MM

50,16

31,309 0,023 228 7,458 91.8 ML/ML

60,19

80,646 0,022 210 7,599 87.7 HM/HL

70,15

90,907 0,019 243 8,414 77.7 HM/ML

80,34

91,184 0,026 251 8,830 78.0 HL/HL

90,25

40,992 0,025 224 7,726 0,0 HL/HM

Lyoph.

0,007 720 8,855 90.7 -

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Page 24: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Global valorization

Exp.Phase I Phase II

Tair Tf Ts* Taire Tf Ts

*

2 5 20 35 2027,5

35

3 5 30 55 4047,5

55

5 20 27,5 35 2027,5

35

Convective lossesViabilit

yPhase I Phase II Total- - -- 97,9

- +++ ++ 93,7

++ ++ ++++ 90,9

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Experiments 2 and 3, spite of their favourable drying rate and good viability results, are discarded because the significant convective losses

Medium thermal levels and low gradients, such as of Exp. 5, are recommended because of its good quality and process efficiency

Page 25: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Conclusions

• Microwave drying has proved to be a good technology for microencapsulated probiotics with high percentage of survival.

• The mathematical model show in the first phase that the diffusivities values are not as high as for the second phase in which a combination of liquid and gas diffusion mechanism take place.

• Considering the viability the best drying conditions would be a medium thermal level and gradient with good results under quality and kinetic criteria.

• In further studies is thought to use a lactobacillus strain applying medium thermal strategies here found as the most adequete.

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Page 26: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

AcknowledgementsGroup at UPV/EHU

Janire MardarasDr. Monika OrtuetaDr. J. Ignacio Lombraña

e-mail: [email protected]

Group at Tecnalia

Dr. Noelia HidalgoDr. M. Carmen Villarán

e-mail: [email protected]

UPV/EHU

The authors are grateful to the Basque Government for the financial support of the study through the Aid (IT801-13) within the program to consolidate Groups (Basque University System) and to the University of the Basque Country (UFI 11/39 UPV/EHU).

Page 27: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. *P.O Box 644. 48080 Bilbao (Spain). Phone +34 94 601 25

[email protected]

5th Euro-Global Summit and Expo on

Food & Beverages June 16 – 18, Alicante, Spain

QUALITY VALORIZATION OF MICROENCAPSULATED PROBIOTICS DEHYDRATED BY MICROWAVE DRYING

THANK YOU FOR YOUR ATTENTION!!

Dr. J. Ignacio Lombrañae-mail: [email protected]

Page 28: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Mass transfer model

z

M

zy

M

yx

M

xD

t

MD1,D2,D3

Boundary conditions:

)exp()( 0 tMMMM eeS (Shivhare 1994)

sph

sphav V

dxdydzzyxM

M

),,(

Page 29: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

Diffusion coefficients and Surface drying coefficient (β)

Exp. βD1(x 10-

8)D2(x 10-

8)D3(x 10-8) Code

1 0.054 3.2 4.8 7.0 MM/MM

2 0.050 4.2 6.0 3.2 MM/ML

3 0.074 6.0 8.0 1.0 HH/HL

4 0.066 2.2 4.2 1.0 ML/MM

5 0.055 5.0 7.2 0.7 ML/ML

6 0.090 6.1 9.1 0.8 HM/HL

7 0.069 3.4 5.6 1.0 HM/ML

8 0.110 3.6 3.4 0.1 HL/HL

9 0.090 5.2 5.0 0.9 HL/HM*Units: β (min -1), D ( m2/min).

Page 30: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

0

1

2

3

4

0 25 50 75 100 125 150

M (g H2O/g d.s.)

time(min)

Exp 1Exp 2Exp 3

I II III

Page 31: J.I. Lombraña Dept. of Chemical Engineering. Faculty of Science and Technology. Universidad del País Vasco. * P.O Box 644. 48080 Bilbao (Spain). Phone

01234560

0.2

0.4

0.6

0.8

1

Exp.2

Exp.9

M [g H2O/g ss]

aw

Phase I Phase II

Phas

e II

I

0

0.2

0.4

0.6

0.8

1

0246

aw

M [g H2O/g ss]

Exp.2

Exp.9

Phase I Phase II

Phase

III