Starch-stearic Acid Complex Development within Single and

Twin Screw Extruders

SANDEEP BHATNAGAR and MILFORD A. HANNA

ABSTRACT
Corn starch was extruded with 4% stearic acid in Brabender single screw
and twin screw laboratory extruders. The screws were cooled and removed and samples were collected from locations along the screws. In
the single screw extruder, starch gelatinization as determined by DSC
and polarized light microscopy started in the compression zone and was
completed in the metering zone. Starch-stearic acid complex formation
as determined by iodine binding capacity and X-ray diffraction started
at the same point as gelatinization and increased to a maximum near the
tip of the screw. In the twin screw extruder, starch gelatinization and
starch-stearic acid complex formation started at a distance of seven screw
diameters and continued from there to the die end.
Key Words: extrusion, screw configuration, starch gelatinization, complexing profile, x-ray diffraction

INTRODUCTION
IN MOST MANUFACTURING of extruded food products, a powdery
mix of raw materials is introduced into a heated barrel of an
extruder. The mixture is transported and compressed in the
screw channel by one or more rotating screws. The specific thermal and mechanical energies introduced into the product cause
the material being transported to be plasticized. Under the conditions of extrusion cooking, and depending on the raw materials
and process variables, raw material transformations and energy
conversion take place that can lead to products of very diverse
natures. The changes of greatest importance include gelatinization of starch, coagulation of proteins, and formation of complexes between amylose portion of starch and lipid and
protein-lipid complexes (Mercier et al., 1980; Harper, 1981; Colonna and Mercier, 1983; Schweizer et al., 1986; Galloway et
al., 1989; Ho and Izzo, 1992; Guzman et al., 1992; Bhatnagar,
1993; Bhatnagar and Hanna, 1994a, b).
Several studies have been devoted to understanding amyloselipid complex formation (Mikus et al., 1946; Osman et al., 1960;
Gray and Schoch, 1962; Krog, 1971; Van Lonkhuysen and
Blankestijn, 1974; Hoover and Hedziyev, 1981; Hahn and Hood,
1987). Amylose-lipid complexes can be prepared by the addition
of a complexing agent to a hot aqueous solution of starch. During cooling of the hot solution, the amylose constituent of the
starch separates in a crystalline complex which can be recovered
readily. According to Kugimiya et al. (1980), complex formation takes place immediately after gelatinization in an exothermic process as observed in DSC experiments. Temperature
studies on fatty acid-starch complexing have shown that an increase in temperature results in decreased swelling power, soluble starch, and Brabender peak viscosity, all of which have
been attributed to increased complex formation (Gray and
Schoch, 1962). Prior to gelatinization, starch has limited binding
capacity for lipid because most of the lipid in the system is
unable to come into contact with the starch. As the starch is
dispersed, the amylose becomes available for complexation.
However, for a process such as extrusion there is an optimum
temperature for complexation which depends on fatty acid chain
The authors are respectively Post Doctoral Research Associate
and Professor, Department of Biological Systems Engineering,
University of Nebraska, Lincoln, NE 68583-0726.

length (Bhatnagar, 1993) and above and below that temperature

there is a decrease in lipid binding (Bhatnagar and Hanna,
1994b).
Other studies have reported the effect of complex formation
on physical and chemical properties such as expansion ratio,
bulk density, water solubility and iodine binding capacity of
starches during extrusion cooking (Mercier et al., 1979, 1980;
Colonna and Mercier, 1983; Schweizer et al., 1986; Galloway
et al., 1989; Bhatnagar, 1993; Bhatnagar and Hanna, 1994a, b).
Increased complexing resulted in decreased expansion ratio, water solubility and iodine binding capacity and increased bulk
density. Asp and Bjorck (1984); Rao and Artz (1989) and Artz
et al. (1992) reported decreases in lipid stability with increases
in extrusion temperature. Mustakas et al. (1970) reported that a
shorter residence time in the extruder reduced the amount of
oxidation of lipids during storage.
Meuser et al. (1987) reported that the degree of complexing
increased as the specific mechanical energy (SME) and product
temperature increased up to a maximum value. Beyond that the
degree of complexation decreased with further increases in combined energy input. Colonna and Mercier (1983), however, suggested that lipids acted as lubricants in extrusion while
Bhatnagar (1993) concluded that each type of lipid had a distinct
effect. This generally should reduce the specific mechanical energy input.
The applied energy causes several changes in the material
being processed in the extruder. During the first few seconds of
transportation in the barrel, water diffuses into the starch granules. The degree of fill of the screw chamber in this first stage
is rather low. Therefore, only a slight increase in temperature
of the hydrated product takes place during its transportation to
the shearing and melting zones. As the product enters the melting zone, compression of the starch granules makes them deform, melt, and lose their crystalline regions. Starch leaving the
melting zone is usually completely gelatinized. Therefore, it is
hypothesized that formation of complex should start in an extruder after sufficient energy has been provided to plasticize the
material. Knowing the point inside the extruder at which complex formation is initiated and how the degree of complexing
varies along the length of the extruder would be useful in assessing how ingredients such as flavors and other organic additives may form helical inclusion complexes. It also would be
useful in determining the appropriate point of injection of such
compounds when it is desirable to have shorter residence time,
to avoid premixing with other ingredients, to avoid overexposure to elevated temperature and pressure or to have shorter
residence time. Therefore, our objective was to observe and
compare starch gelatinization and lipid complexing inside single
and twin screw extruders.
MATERIALS & METHODS
NORMAL CORN STARCH containing 25% amylose (Table 1) was obtained
from American Maize Products Co. of Hammond, IN. Fine starch powder was granulated prior to extrusion to facilitate feeding. Stearic acid
(C18:0, +99% purity) was obtained from Humko Chemical Co. of
Memphis, TN.
Extrusions were carried out in a laboratory scale Model 2802 single
screw extruder and Model TSM twin screw extruder (C.W. Brabender

778JOURNAL OF FOOD SCIENCEVolume 61, No. 4, 1996

Fig. 1Screw configuration for single screw extruder and location of sampling points.

Fig. 3Samples collected from different locations in a single

screw extruder. Feed zone (I), compression zone (II), metering
zone (III), end of metering zone (IV), mixing zone (V), tip of screw
(VI), die (VII) and after die (VIII).

Fig. 2Screw configuration for twin screw extruder and location

of points sampling.
Table 1Proximate analysis of corn starcha
Total amylose (% d.b.)
Protein (% d.b.)
Phosphorus (mg/100 g)
Lipid (g/100g)
Free Lipid
Bound Lipid
Moisture (% d.b.)
Ash (g/100 g)

25.0
0.3
14.2
0.07
0.03
9.5
0.2

a As provided by the manufacturer

Table 2Location of various zones and points of sampling in a single

screw extruder
Sample
I
II
III
IV
V
VI
VII

Description
Unextruded starch-stearic
acid mixture
Feed zone
Compression zone
Metering zone
Mixing section
Tip of screwb (exit)
Before die nozzle

Location from feed enda (D)

0 - 6D (3D)
6D - 9D (7.5D)
9D - 15.6D(12.3D)
15.6D - 20D (15.6D and 20D)
21D
23D

a Values in parenthesis indicate the points in screw diameters (D) from which samples

were collected where D 5 19 mm.

b Even though the barrel length was 20D, the tip of the screw extended 1D beyond the

barrel. Similarly, the die nozzle was located at a distance of 23D from the feed end.

Inc., South Hackensack, NJ). The single screw extruder had a screw of
20:1 length to diameter ratio, a 3:1 compression ratio and a mixing
section located just before the tip of the screw (Fig. 1). The feed zone
was maintained at 707C. The other zones were maintained at 1407C. The
twin screw extruder had 2 universally single flighted counter-rotating
intermeshing screws of 42 mm diameter with interrupted flight mixing
zones (Fig. 2). The barrel had three electrically heated barrel zones which
were maintained at 70, 140 and 1407C. The screw speed and moisture
content in both cases were 140 rpm and 22% (dry weight basis), respectively. Starch and stearic acid (4% starch dry weight basis) were
blended in a Hobart mixer. The appropriate amount of water was then
added. The mixture was allowed to equilibrate for 16 hr at '237C. These
conditions were based on research on optimization of process conditions
for amylose-lipid complexing (Bhatnagar, 1993; Bhatnagar and Hanna,
1994b). The experiment was replicated twice.
The experimental technique used for collecting samples was similar
to that reported by Tadmor and Klein (1970 ) who studied melting of
plastic polymers inside an extruder. The basic concept was to feed a
mixture of starch and stearic acid into the extruders. When steady state

Fig. 4Samples collected from different locations in a twin

screw extruder. At feed port (I), 2.8D (II), 4D (III), 5.5D (IV), 7.1 D
(V), 8.3D (VI), die (VII) and after die (VIII).
Table 3Location of the points of sampling in a twin screw mixera
Sample
I
II
III
IV
V
VI
VII

Location from feed end (D)

Unextruded starch-stearic acid mixture
2.8D
4.0D
5.5D
7.1D
8.3D
10D

a The barrel length was 5.7D. The total length of the system was 10D including the

die and the nozzle where D 5 50 mm.

was reached, the screw was stopped and cooled down by blowing ambient air through the heating/cooling jackets on the extruder barrels
thereby solidifying the biopolymers in place. If cooled quickly enough,
the properties of the product in the extruder would be fixed for later
evaluation. When the screw and the solidified mixture was pushed out
of the barrel (Fig. 1, 2) the mixture could be carefully peeled off the
screw to provide samples at different locations along the extruder barrel
(Table 2 and 3). Cooling of the screws, their removal and sample collection were done in 30 min. Therefore, we assumed that retrogradation
was negligible. Collected samples were then dried at 407C in a forced
convection oven for 12 hr and stored in glass bottles until analyzed.
Degree of gelatinization was determined by differential scanning calorimetry (DSC). DSC thermograms were obtained with a Dupont 2000

Volume 61, No. 4, 1996JOURNAL OF FOOD SCIENCE779

STARCH LIPID COMPLEX DEVELOPMENT WITHIN EXTRUDERS . . .

Fig. 5Degree of gelatinization and loss of birefringence as a function of distance from feed end of single screw extruder (A) and
twin screw extruder (B); and peak height for peak at 2u 5 19.5& and iodine binding capacity for a single screw extruder (C) and a
twin screw extruder (D).

Thermal analyzer system with a 910 cell base (TA Instruments, PA).
The instrument was calibrated with indium using an empty pan as reference. Sample preparation involved weighing 2 to 3 mg of ground sample into a tared DSC pan. Enough water was added using a micro syringe
to provide 20% solids in the mixture. DSC pans were hermetically sealed
and heated from room temperature to 1207C at 107C/min in the presence
of N2, and DH values were recorded. Degree of gelatinization was calculated as
(DHNative Starch 2 DHSample)
3 100
DHNative Starch
where DH was heat of gelatinization determined from endotherm.
The unmodified fraction also was determined by counting the birefringent and gelatinized granules in selected samples using a polarizing
microscope. The granules which had partially lost birefringence were
counted as gelatinized. To facilitate microscopic measurements, samples
were stained with Congo red dye.
Complex formation between the starches and stearic acid during extrusion was studied using powder X-ray diffraction. All samples were
defatted using petroleum ether in a Soxtec fat extractor (Tecator, Inc.,
Germany) to remove free stearic acid (Bhatnagar and Hanna, 1994a) and
then dried at 407C to 10% (d.b.) moisture in a forced air convection
oven. Samples of native starch, extruded starch and starch extruded with
stearic acid were analyzed using a Scintag Model Pad (V) X-ray diffractometer (Scintag Inc., Sunnyvale, CA), equipped with a graphite
monochrometer and a scintillation detector (Bhatnagar and Hanna,
1994a). The X-ray source was CuKa radiation with a wavelength of
, 40 kV and 30 mA. With u being the angle of diffraction, data
1.5406 A
were collected from 2u 5 0 to 307 with a step width of 0.027 and step
time of 0.4 sec. The value of 2u for each identifiable peak on the diffractograms was estimated and crystal d spacings were calculated using
Braggs law. Complex formation also was confirmed by determining the
iodine binding capacity of samples as outlined by Schoch (1964) after
removal of the free stearic acid (Bhatnagar and Hanna, 1994a, b).
%gelatinized 5

RESULTS & DISCUSSION

THE SAMPLES collected from different locations along the extruder screws (Table 2 and 3) were compared (Fig. 3 and 4). The

single and twin screw extruders processing conditions represented extremes. The single screw had extruder compression and
mixing sections while the twin screw was uniformly flighted. In
the single screw extruder, the appearance of the starch-stearic
acid mixture started changing after the feed zone (Fig. 3 I). The
mixture started to melt slightly in the compression section (Fig.
3 II) and was completely melted by the end of the metering
section. The samples collected from this section at a distance of
12D from feed end were glossy and fused masses. The degree
of gelatinization was measured by DSC (Fig. 5A) and loss of
birefringence as a function of distance from the feed end expressed in barrel diameters. At a distance of 10D only 50% of
the starch was gelatinized compared to 80% gelatinized at 15D.
The loss of birefringence, however, was '100% at a distance
of 15D.
In the case of the twin screw extruder, the mixture appeared
glossy at a distance of 7D from the feed end (Fig. 4 IV) which
was near the end of the screw flights. The degree of starch
gelatinization in the twin screw extruder was measured as a
function of distance from the feed end (Fig. 5B). In this case,
gelatinization was not completed until the material reached the
die.
In both single screw and twin screw extruders, the gelatinization measured by loss of birefringence indicated complete
starch gelatinization while DSC indicated only 9095% gelatinization. The difference between the results can be attributed to
the fact that DSC measured the melting of crystallites while the
loss of birefringence measured the loss of order (Zobel, 1992).
Complete loss of birefringence or order would be expected for
extruded products because of the shearing involved inside the
extruder but presence of stearic acid may have affected the crystallite melting.
An enzymatic starch gelatinization measurement, such as that
of Chiang and Johnson (1977 a, b), could not be used because
the starch was extruded with stearic acid which formed com-

780JOURNAL OF FOOD SCIENCEVolume 61, No. 4, 1996

Fig. 6X-ray diffractograms of samples collected from different

locations in a single screw extruder. Unextruded starch (A), feed
zone (B), compression zone (C), metering zone (D), mixing zone
and die (F).

Fig. 7X-ray diffractograms of samples collected from different

locations in a single screw extruder. Feed port (A); distances of
2.8D (B) and 7.1D (C); and die (D).

plexes with amylose. This complex formation has been reported

to decrease the susceptibility of starch to enzymes (Holm et al.,
1983; Eliasson and Krog, 1985). Based on the X-ray diffractograms (Fig. 6 and 7) and results of the X-ray diffraction studies
of gelatinization by Priestley (1975) and Zobel et al. (1988), it
is apparent that the starch was gelatinized. Thus, starch was
gelatinized in the metering section at a distance of '15D from
the feed end in the single screw extruder and at '9D in the
twin screw extruder. Therefore, the remaining barrel length in
the single screw extruder could be used for injection of CO2 to
control product density, heat sensitive colors and flavors, monomers to initiate grafting or for cooling to control density.
The complex formation between amylose and stearic acid was
confirmed by X-ray diffraction and iodine binding capacity. The
X-ray diffraction patterns for samples collected from the single
and twin screw extruders (Fig. 6 and 7) show a V pattern with
peaks at 2u 5 12.6 and 19.57. These patterns were compared to
those reported by Zobel (1964, 1988), Mercier et al. (1979,
1980) and Bhatnagar and Hanna (1994a). These patterns confirmed helical conformation of amylose molecules with six glucose residues per turn.
In the single screw extruder, the first appearance of the V
pattern, corresponding to amylose-stearic acid complex formation, was observed for samples collected from the beginning of
the metering section of the extruder. Thereafter, peak heights in
the V pattern increased as distance from the feed end of the
extruder increased. The peaks also became sharper and more
distinct as compared to their first appearance. For the twin screw
extruder, the first V pattern was observed at 7D from the feed
end. The peak heights of the V pattern increased thereafter and
peaks became much more distinct as the distance from the feed
end increased similar to that observed in the single screw extruder. The d spacings and peak heights were compared (Table 4,
5) for samples from different locations. The peak height for the
) and iodine binding capacity of
peak at 2u of 19.57 (d 5 4.5 A
starch samples from different locations in the single and twin
screw extruders were compared (Fig. 5C, D) as a function of
distance from the feed end. The decrease in iodine binding with
increasing peak height and complexing was evident in both
cases. It also was evident that the majority of the complexing
took place in the metering section for the single screw extruder
and near the die in the twin screw extruder.
These results indicate that in both extruders, the binding of
stearic acid began as soon as starch started gelatinizing. This
corresponded to the beginning of the metering section in the
single screw extruder and at a distance of 7D from the feed end
in the twin screw extruder. The starch granules were com-

Table 4X-ray diffractogram peak heights and d spacings for samples collected from various locations in a single screw extruder
Peak at 2U 5 12.6&
Sample
3D
7.5D
12.3D
20D
Die

d spacing
A
N.P.b
6.930
6.903
6.903
6.903

Peak at 2U 5 19.5&

Peak heighta

d spacing
A

Peak heighta

N.P.
2.1
3.1
4.1
4.1

N.P.
4.503
4.488
4.532
4.503

N.P.
2.5
3.5
5.5
5.6

a Arbitrary units.
b N.P.No peak was observed.

Table 5X-ray diffractogram peak heights and d spacings for samples collected from various locations in a twin screw extruder
Peak at 2U 5 12.6&
Sample
3D
7.1D
8.3D
Die

d spacing
A
N.P.b
6.903
6.903
6.903

Peak at 2U 5 19.5&

Peak heighta

d spacing
A

Peak heighta

N.P.
1.7
3.9
4.1

N.P.
4.489
4.503
4.503

N.P.
3.0
5.6
5.6

a Arbitrary units.
b N.P.No peak was observed.

pressed, deformed and started to melt and lose their crystalline

regions somewhere near the metering zone. The starch was gelatinized as it left the metering zone as indicated by loss of
birefringence. Amylose-stearic acid complex formation also
took place in this zone. This confirmed work of Kugimiya et al.
(1980) who used DSC and concluded that the complex formation took place when starch was gelatinizing and free lipid was
present. Another point of interest was that the peak heights on
the X-ray diffraction patterns, which represented the degree of
complexing, increased to a maximum near the exit end of the
screw in both extruders. Thus, lipids and flavor compounds,
which may be affected by heat, could be injected near the die
end to avoid thermal changes (Rao and Artz, 1989). Lipids also
exhibit a lubricating effect (Colonna and Mercier, 1983) inside
the extruder. This problem is more pronounced in the case of
single screw extrusion where the reduction in friction could affect the feeding of the material. Hence, injection of lipids near
the die may be beneficial as it would avoid reduction in friction
in the feed section.
Comparing the single and twin screw extruder configurations,
similar peak heights and similar degrees of complexing with 4%
stearic acid were observed for the two types of extruders. A

Volume 61, No. 4, 1996JOURNAL OF FOOD SCIENCE781

STARCH LIPID COMPLEX DEVELOPMENT WITHIN EXTRUDERS . . .

detailed analysis of these results is confounded by the difference
in flight depths, mixing vs plug flow situations and other factors
which influence shearing and heat transfer. Samples collected
from the dies of both the single and twin screw extruders contained unbound stearic acid. Thus, the extrusion process did not
complex all of the 4% stearic acid even though Hahn and Hood
(1987) using an equilibrium dialysis technique reported that
5.25% stearic acid could be complexed with starch.
CONCLUSIONS
BOTH GELATINIZATION and complex formation were functions
of distance from the feed end. In the single screw extruder,
complex formation started in the compression section (distance
of 7.5D from feed end) and continued up to the die section with
the majority of complexing taking place in the metering section
(9D15.6D). In the twin screw extruder, complex formation was
evident at 7D from the feed end and continued up to the die
section.
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Ms received 11/7/95; revised 3/16/96; accepted 3/21/96.

Journal Series No. 11336, Institute of Agricultural and Natural Resources, University of
Nebraska, Lincoln.

GLUTATHIONE PEROXIDASE IN FISH. . .From page 735

Nakano et al. (1992) reported that salmon muscle glutathione
peroxidase activity increased during 47C storage and proposed
that the enzyme protects fish muscles from oxidative deterioration during storage and processing. In our study, however, the
fish muscle enzyme activity decreased during the 5-days-storage
at 47C, and no GSH (enzyme substrate) was detected in the
muscles stored for 5 days. During storage, lipid hydroperoxides
in the fish muscles increased substantially. These results suggest
that the increase in lipid hydroperoxides is due to losses in both
enzyme and GSH, and did not confirm the hypothesis of Nakano
et al. (1992). To demonstrate more clearly that the enzyme can
protect fish muscle from oxidative deterioration during storage,
further biochemical studies are needed.
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Ms received 11/16/95; revised 2/11/96; accepted 2/18/96.

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782JOURNAL OF FOOD SCIENCEVolume 61, No. 4, 1996

We thank Miss Kazumi Yokoyama for technical assistance.