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Der ganzheitliche Ansatz in der
Produktentwicklung
Bildung von Karamell-Flavour
durch Extrusion
Imre BlankNestle PTC Orbe
IVV Jahrestagung, Freising, 4-5. Juni 2008
IVV meeting / June 6, 2008 / I. Blank 2
Flavour is one of the major drivers of consumer preference
However, there are many other factors of similar importance
Colour, shape, texture,
Nutritive value, safety, Convenience, packaging, …
Flavouring can be achieved by- Adding finished flavours,
- Generating flavours upon food processing, e.g. extrusion
Louis-Leopold Boilly, Les Cinq Sens (The Five Senses), 1823.
IVV meeting / June 6, 2008 / I. Blank 3
Flavour generation upon extrusion
Extrusion� Heat load (T, t)� Screw speed, SME� Moisture� Number of barrels � Slurry vs. dry addition� …
Recipe� Ingredients� Specific precursors� Concentration, ratio� Catalyst� pH� …
Highly complex system 1. Model productManifold interactions & variability 2. Target product
Effects difficult to predict Systematic approach Experimental design
Product characterisation Sensory evaluationVolatiles/non-volatiles analysesChemical/physical measurements
IVV meeting / June 6, 2008 / I. Blank 4
Generation of caramel-type flavournotes upon extrusion
Objective:
� Identify conditions favouring the transformation of rhamnose into furaneol - a caramel-like smelling compound
� Extruded product: Effect of extrusion parameters and recipe composition on furaneol formation from rhamnose and lysine
Optimised recipe and processing conditions favouring the formation of caramel flavour upon extrusion of rice flour
NH2 OH
O
NH2 O
OHO
CH3
CH3
+Recipe/Process
parameters
IVV meeting / June 6, 2008 / I. Blank 5
� Odour and taste:
� Odour threshold:
� Formation:
� Properties:
Target compound: Furaneol(4-Hydroxy-2,5-dimethyl-3(2H)furanone)
• white to yellow powder
• sensitive to oxidation
� Key flavour: • Fruits strawberry and pineapple
• Roasted products coffee, almonds, cereals
• depending on pH
• 21-158 µg/kg water
O
OHO
CH3
CH3
• degradation of 6-deoxy-sugars
in the presence of amino acids
• fruity, caramelized, sweet
IVV meeting / June 6, 2008 / I. Blank 6
Thermally induced formation of furaneol from sugars & derivatives
O
OHO
CH3
CH3
Amadori compounds
CH2- NH-CH-COOH
C=O
(CH-OH)3
CH2-OH
R
Hexose phosphates
CHO
CH-OH
(CH-OH)3
CH2-O- P
Hexose sugars
CHO
CH-OH
(CH-OH)3
CH2-OH
6-Deoxyhexose
CHO
CH-OH
(CH-OH)3
CH3
Sugar fragments
C3 + C3
Strecker-assisted
chain elongation
C5 + C1
IVV meeting / June 6, 2008 / I. Blank 7
Experimental setup: Key product attributes
affected by recipe and extrusion parameters
Recipe parameters • pH
• Ratio Rha/Lys
• Phosphate
Extrusion parameters• Moisture levels
• Screw Speed
• Temperature
• Residence time
• Slurry vs. dry
Mixing
Extrusion
Drying
Milling
Final product
Product characterisation
• Texture
• Crispness
• Colour
• Flavour
• Acrylamide
• Starch degradation
• Granulometry
• Viscosity
• Sensory
Fractional factorial design:- 32 instead of 576 trials
Modelling furaneol yield & rhamnose degradation by estimating
- all main effects and
- two-factor interactions
of 3 recipe & 5 process parameters
500400300Screw speed (rpm)
150135120Temp. (°C)
0.1340.035PO4 (mol/kg)
232017Moisture (%)
SlurryDryAddition
75Barrel length
3:13:0Rha:Lys
7.76.4pH
IVV meeting / June 6, 2008 / I. Blank 8
Holistic approach: Analytical characterisation
of samples from experimental design
List of analysis:• Residual rhamnose (HPLC/DAD)
• Furaneol (GC/MS)
• Acrylamide (HPLC/MS)
• Chemical composition (NIR)
• Moisture (MNR)
• Molecular weight profile of starch (GFAS = Gel Filtration Analysis of Starch)
• Molecular weight profile of debranched starch (SEC = Size Exclusion
Chromatography)
• Molecular weight profile of proteins (HPSEC = High Performance Size
Exclusion Chromatography)
• Colour
• Viscosity (rheometer, RVA profile)
• Granulometry (laser diffraction)
• Texture (X-ray tomography)
• Porosity (cells size & cell walls distributions, degree of anisotropy)
• Crispiness (average drop off, force Max)
• Sensory evaluation
Flavour ⇔ Recipe/process parameters ⇔ Other key product attributes
IVV meeting / June 6, 2008 / I. Blank 9
• Trained panel (14 panelists)
• Product– Extruded powder (85%)
– Sugar (15%)
• Reconstitution– 12.4g product
– 100mL milk at 70°C
• 32 Products evaluated vs. reference
• Identification of statistically relevant
trends
Parameters units Low Medium High
pH 6.4 7.7
Rha:Lys 3:0 3:1
Phosphate mol/kg 0.035 0.134
Moisture % 17 20 23
Screw speed rpm 300 400 500
T °C 120 135 150
length barrel short long
Addition dry slurry
Sensory assessment: Reconstituted
products from experimental design
-6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6
tEasySwallow
aLump
tSmooth
Burnt
Nutty
aDark
Caramel
Toasted
Processy
Off
Overall
acid
WholeGrain
Mushroom
astringent
bitter
aftertaste
t1Thick
tThick
tFluffy
t1Wettability
tSemolina
Cooked
Milky
Rice
Vanilla
sweet
Range covered by A01-A32 (vs. REF)
Fla
vo
r
Textu
re &
Ap
peara
nce
Range of sensory attributes
Wide diversity of sensory perception
IVV meeting / June 6, 2008 / I. Blank 10
0
4
8
12
16
20
20 30 40 50 60 70 80 90 100
SME measured / Wh/kg
Fu
ran
eo
l d
ry /
mo
l%
Correlation matrixNo correlation between furaneol level and SME
IVV meeting / June 6, 2008 / I. Blank 11
Correlation matrix
Furaneol vs SME
SME measured
SME calculated
Visco5min
ViscoMax
ViscoMaxTime
Visco5/3min
L
ab
C
h
Rha extRha dry
Furaneol ext
Furaneol dry
0
4
8
12
16
20
20 30 40 50 60 70 80 90 100
SME measured (Wh/kg)
Fu
ran
eol d
ry (
mo
l%)
Acrylamide
SME is negatively
correlated with viscosity
Furaneol is positively
correlated with the
degradation of rhamnose
and colour development
IVV meeting / June 6, 2008 / I. Blank 12
Sensory evaluationLink between sensory data and SME or Furaneol
sweet
VanillaRice
Milky
Cooked
tSemolina
t1Wettability
tFluffy
tThick
t1Thick
aftertaste
bitter
astringent
Mushroom
WholeGrain
acid
Overall
OffProcessy
Toasted
Caramel
aDark
Nutty
Burnt
tSmooth
aLump
tEasySwallow
Furaneol
SME
� Furaneol is related to odour,
flavour, and taste attributes
High � caramel, bitter/astringent,
strong overall/aftertaste,
burnt/nutty/toasted and
dark color
Low � mild notes, sweet, vanilla,
milky, cooked, rice
� SME is related to texture and
appearance
High � smooth, easy to swallow
Low � thick, semolina, wetability
IVV meeting / June 6, 2008 / I. Blank 13
Furaneol formation Free AA, moisture, T and phosphate are most critical
-6 -4 -2 0 2 4 6
pH 6.4pH 7.7
Rha:Lys 3:0Rha:Lys 3:1
Phosphate 0.035 mol/kgPhosphate 0.134 mol/kg
17% H2O20% H2O23% H2O
300 1/min400 1/min500 1/min
120 °C-Long120 °C135 °C150 °C
DrySlurry
Furaneol ext / mol% Furaneol dry / mol% Conversion of rhamnose to furaneol can be modulated through
changes of extrusion and/or recipe parameters
-6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6
tEasySwallowaLump
tSmooth
BurntNutty
aDarkCaramelToasted
ProcessyOff
Overallacid
WholeGrainMushroomastringent
bitteraftertaste
t1ThicktThicktFluffy
t1WettabilitytSemolina
CookedMilkyRice
Vanillasweet
Range covered by A01-A32 (vs. REF)
Fla
vo
r
Se
ns
ory
imp
ac
t
Enhanced with furaneol
Reduced with furaneol
IVV meeting / June 6, 2008 / I. Blank 14
Effect of recipe/extrusion parameters Furaneol vs SME
pH 6pH 7
Rha:Lys 3:0
Rha:Lys 3:1
Phosphate low
Phosphate high
17% H2O
20% H2O
23% H2O
300rpm
400rpm
500rpm
120°C-Long
120°C135°C
150°C
Dry
Slurry
-4
-3
-2
-1
0
1
2
3
4
-20 -15 -10 -5 0 5 10 15 20
SME-measured
%F
ura
ne
ol-
dry
Temperature affects
both furaneol and SME
Free amino acid and
phosphate affect
furaneol, but not SME
Moisture affects both
furaneol and SME
IVV meeting / June 6, 2008 / I. Blank 15
Colour generation
-6 -5 -4 -3 -2 -1 0 1 2 3 4 5 6
tEasySwallowaLump
tSmooth
BurntNutty
aDark
CaramelToasted
ProcessyOff
Overallacid
WholeGrainMushroomastringent
bitteraftertaste
t1ThicktThicktFluffy
t1WettabilitytSemolina
CookedMilkyRice
Vanillasweet
Range covered by A01-A32 (vs. REF)
Se
ns
ory
imp
ac
t
Colour range
Colour development through extrusionModulate colour in product through recipe
Browning reactions
-6 -4 -2 0 2 4 6
pH 6pH 7
Rha:Lys 3:0Rha:Lys 3:1
Phosphate lowPhosphate high
17% H2O20% H2O23% H2O
300rpm400rpm500rpm
120°C-Long120°C135°C150°C
DrySlurry
Colour (C)
** Lysine
* High pH
Ke
y p
ara
me
ters
Light Dark
pH 6Rha/Lys 3:0
pH 7Rha/Lys 3:1
IVV meeting / June 6, 2008 / I. Blank 16
Acrylamide Temperature is most critical
-75 -50 -25 0 25 50 75
pH 6.4
pH 7.7
Rha:Lys 3:0
Rha:Lys 3:1
Phosphate 0.035 mol/kg
Phosphate 0.134 mol/kg
17% H2O
20% H2O
23% H2O
300 1/min
400 1/min
500 1/min
120 °C-Long
120 °C
135 °C
150 °C
Dry
Slurry
Acrylamide
-6 -4 -2 0 2 4 6
pH 6.4pH 7.7
Rha:Lys 3:0Rha:Lys 3:1
Phosphate 0.035 mol/kgPhosphate 0.134 mol/kg
17% H2O20% H2O23% H2O
300 1/min400 1/min500 1/min
120 °C-Long120 °C135 °C150 °C
DrySlurry
Furaneol ext / mol% Furaneol dry / mol%
17-235 ppb
IVV meeting / June 6, 2008 / I. Blank 17
SME Temperature, moisture, screw speed are most critical
-15 -10 -5 0 5 10 15
pH 6.4pH 7.7
Rha:Lys 3:0Rha:Lys 3:1
Phosphate 0.035 mol/kgPhosphate 0.134 mol/kg
17% H2O20% H2O23% H2O
300 1/min400 1/min500 1/min
120 °C-Long120 °C135 °C150 °C
DrySlurry
SME measured / Wh/kg SME calculated / Wh/kg
Higher SME is achieved with low
moisture, high screw speed, low
temperature and long extruder.
No effect of recipe parameters on SME
IVV meeting / June 6, 2008 / I. Blank 18
Structure and Texture Moisture and temperature are most critical
-1500 -1000 -500 0 500 1000 1500
pH 6.4pH 7.7
Rha:Lys 3:0Rha:Lys 3:1
Phosphate 0.035 mol/kgPhosphate 0.134 mol/kg
17% H2O20% H2O23% H2O
300 1/min400 1/min500 1/min
120 °C-Long120 °C135 °C150 °C
DrySlurry
Visco5min / mPas ViscoMax / mPas
-15 -10 -5 0 5 10 15
Cell walls / µm
Structure = f (SME)Texture = f (SME)
IVV meeting / June 6, 2008 / I. Blank 19
StructureWide variety of structures obtained
-20 -10 0 10 20
Rha:Lys 1:0Rha:Lys 3:1
0.035 mol/kg PO40.134 mol/kg PO4
17% H2O20% H2O23% H2O
300 1/min400 1/min500 1/min
120 °C-Long120 °C135 °C150 °C
DrySlurry
Main effect
Cell walls (um)
0
200
400
600
800
1000
1200
70 75 80 85 90
Porosity (%)
Mean
cell s
ize (
um
)
12 mm
IVV meeting / June 6, 2008 / I. Blank 20
Long ChainDP~50
Short ChainDP~25
Rice Flour
Moisture % 8-13
Starch %d.b. 88-92
Total fibers %d.b. 0.3-1
Proteins %d.b. 6-9
Fat %d.b. 0.5-1
Ash %d.b. 0.3-1
A17
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular weight
Ca
rbo
hy
dra
tes (
g/1
00g
)
Total Amylopectin Intermediate1
Intermediate2 Amylose
A31
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular w eight
Ca
rbo
hy
dra
tes (
g/1
00g
)
Total Amylopectin Intermediate1
Intermediate2 Amylose
A28
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular w eight
Ca
rbo
hyd
rate
s (
g/1
00g
)
Total Amylopectin Intermediate1
Intermediate2 Amylose
A04
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular w eight
Carb
oh
yd
rate
s (
g/1
00
g)
Total Amylopectin Intermediate1
Intermediate2 Amylose
Amylopectin
High MW
Am
ylo
pe
cti
n,
hig
h M
W I
nte
rme
dia
te d
ep
oly
me
rize
d
Lo
wM
W In
term
ed
iate
ge
ne
rate
d, a
mylo
se
co
ns
tan
t
Low MW
Amylose
SME 92 SME 35
Texture: Starch degradation Depolymerisation of amylopectin increases with SME
IVV meeting / June 6, 2008 / I. Blank 21
A17
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular weight
Ca
rbo
hy
dra
tes (
g/1
00g
)
Total Amylopectin Intermediate1
Intermediate2 Amylose
A31
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular w eight
Ca
rbo
hy
dra
tes (
g/1
00g
)
Total Amylopectin Intermediate1
Intermediate2 Amylose
A28
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular w eight
Ca
rbo
hyd
rate
s (
g/1
00g
)
Total Amylopectin Intermediate1
Intermediate2 Amylose
A04
0
10
20
30
40
50
60
70
80
90
100
1000 10000 100000 1000000 10000000 100000000
Molecular w eight
Carb
oh
yd
rate
s (
g/1
00
g)
Total Amylopectin Intermediate1
Intermediate2 Amylose
Amylopectin
High MW
Am
ylo
pe
cti
n,
hig
h M
W I
nte
rme
dia
te d
ep
oly
me
rize
d
Lo
wM
W In
term
ed
iate
ge
ne
rate
d, a
mylo
se
co
ns
tan
t
Low MW
Amylose
SME 92 SME 35
0
20
40
60
80
100
0 50 100
SME
Sta
rch
(%
)
Amylopectin
High MW
intermediate
Low MW
intermediate
Starch degradation MW = f (SME)
0
1000
2000
3000
4000
5000
6000
0 2 4 6 8 10 12
Vis
co
sit
y (
mP
a.s
)
Time (min)
SM
E 9
2S
ME
35RVA 50°C, 50rpm
21g+170mL milk
Viscosity = f (MW)
High H2OHigh T
Low H2OLow T
IVV meeting / June 6, 2008 / I. Blank 22
Conclusions
Critical parameters for generation of furaneol from rhamnose during extrusion:
• Furaneol generation is affected both by recipe parameters (Lys, PO4) and
extrusion parameters (T, moisture)
• Recipe parameters permit furaneol modulation w/o impact on texture
• Lower pH will limit colour and acrylamide development w/o affecting furaneol
formation
• Addition of amino acid will enhance furaneol while limiting acrylamide formation
• Temperature and moisture affect both furaneol formation and texture (→ SME)
Full factorial design
IVV meeting / June 6, 2008 / I. Blank 23
� Hélène Chanvrier PTC Orbe Structure, texture
� Tomas Davidek PTC Orbe Flavour, acrylamide
� Valérie Leloup PTC Orbe Macromolecular chemistry
� Werner Pfaller PTC Orbe Extrusion
� Andreas Rytz NRC Lausanne Experimental design
� Silke Illmann Univ. Karlsruhe Diploma work
� Claudia Leeb Univ. Karlsruhe Extrusion
� Heike Schuchmann Univ. Karlsruhe Extrusion
Thanks to…
………… and to you for your kind attention !and to you for your kind attention !and to you for your kind attention !and to you for your kind attention !
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