Effect of heat moisture treatment and annealing on physicochemical properties of red sorghum starch

African Journal of Biotechnology Vol. 4 (9), pp. 928-933, September, 2005
Available online at http://www.academicjournals.org/AJB
ISSN 1684–5315 © 2005 Academic Journals





Ful Length Research Paper

Effect of heat moisture treatment and annealing on
physicochemical properties of red sorghum starch

Kayode O. Adebowalea, Bamidele I. Olu-Owolabi a, Olufunmi O. Olayinkaa, and Olayide S.
Lawalb

aDepartment of Chemistry, University of Ibadan, Ibadan, Nigeria.
bDepartment of Chemical Science, Olabisi Onabanjo University, Ago-Iwoye, Nigeria.

Accepted 14 June, 2005

Red sorghum starch was physically modified by annealing and heat moisture treatment. The swelling
power and solubility increased with increasing temperature range (60-90°), while annealing and heat-
moisture treatment decreased swelling power and solubility of starch. Solubility and swelling were pH
dependent with higher values obtained at pH 12 in both native and modified starches. Water absorption
capacities of both annealed and heat-moisture treated starches increased with increasing levels of
moisture treatment while highest value was observed in annealed starch. Oil absorption capacity of
annealed starch was increased which was contrast to heat-moisture treated starches which decreased
from 160 glg in native starch to 140 glg in HMR18 and HMR27. Pasting analysis in the Rapid Visco
Analyser (RVA) revealed that both annealing and heat-moisture treatment increased pasting
temperature, while alkaline water retention improved after physical modification.

Key words: Red sorghum starch, heat moisture treatments, annealing, functional properties.


INTRODUCTION

Starches are the principal food reserve polysaccharides
Hemisphere. It contains a high percentage of starch (65–
in the plant kingdom. They form the major source of
76%) and protein (11.6%). However, it contains some
carbohydrates in human diet and are therefore of great
antinutritional components that could limit its direct
economic importance. Starches obtained from grains,
consumption in foods and feeds. Hence, the need to
tubers and roots have been consumed as food for many
process it very wel (D’mel o and Walker, 1991).
centuries (Jones, 1983). Starch is a very versatile raw
Depending on the botanical source, starches present
material with a wide field of applications. The growing
specific physicochemical and functional properties. The
demand of starches for the modern food industry has
main functional properties of native starches are their
created interest for new sources of this polysaccharide. It
good thickening and gel ing properties, which makes
occurs in granular form and the shapes of the granules
them excel ent ingredients for the manufacture of foods
are characteristic of the source of the starch. Starch
such as custards, porridges, puddings, cookies and
granule can be separated into two distinctly different
sausages (Pomeranz, 1991).
components, amylose and amylopectin (Hoover et al.,
The molecular arrangement in a starch granule can be
1991).
altered by various physical treatments. Annealing and
Sorghum is cultivated in the arid regions of the world. It
heat-moisture treatments (HMT) are two common
has a high agronomic potential even under adverse
physical means by which the treated starch can acquire
tropical conditions, with 49.8% produced in the Western
modified properties without rupturing the granule.

Annealing is general y carried out by heating granule

starch with a large quantity of water at a temperature

below the starch melting point, whereas HMT is carried

out at limited moisture contents (18, 21, 24, and 27%) but
*Corresponding Author’s E-mail: ko.adebowale@mail.ui.edu.ng
at an elevated temperature (Eliasson and Gudmundsson,

1996). These physical treatments can change certain

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Adebowale et al. 929






starch properties using simple and environmental y safe
starch was then dispersed in 50 cm3 of distil ed water using a
processes. The physical properties of a heat-moisture
blender. The resultant slurry was heated at the desired temperature
treated starch depend on the starch origin and treatment
(60, 70, 80, 90oC) for 30 min in a water bath. The mixture was
conditions used.
cooled to 30±2°C and centrifuged (500 rpm, 15 min). Aliquots (5 ml)
of the supernatant were dried to a constant weight at 110°C. The
In previous works, heat-moisture treated starches
residue obtained after drying the supernatant represented the
displayed an increased paste stability and gelatinisation
amount of starch solubilized in water. Solubility was calculated as
temperature, regardless of origin (Abraham, 1993;
g/100 g of starch on a dry weight basis. The residue obtained from
Col ado and Corke, 1999; Donovan et al., 1983; Hoover
the above experiment (after centrifugation) with the water it retained
and Vasanthan, 1994; Lorenz and Kulp, 1982; Stute,
was quantitatively transferred to the clean dried test tube used
1992). Col ado and Corke (1999) treated a sweet potato
earlier and weighed (w2).

starch, and found that the starch paste became short and
Swel ing of starch = w2 – w1/weight of starch.
sheer-stable and the starch gel exhibited marked

increases in hardness and adhesiveness, whereas

annealing increases susceptibility to amylase (Wang et
Effect of pH on swelling and solubility
al., 1997) and changes pasting curves (Jacobs et al.,

To determine the effect of pH on swel ing and solubility of the
1995; Stute, 1992), Chung et al. (2000), reported that
starch, slurries (1%, w/v) were prepared in distil ed water and the
annealing increased the surface hardness of mung bean
pH adjusted to the desired values with 0.1 M HCl or NaOH. The
starch gels, and the hardness.
slurries were then al owed to stand at 30±2°C for an additional 30
The objective of the present research was to determine
min, centrifuged (5000 rpm, 15 min) and the swel ing (1%) and
the impact of HMT and annealing on physicochemical
solubility determined as described above.
properties of red sorghum. The studies involve isolation


of starch, and determination of physicochemical
Oil and water absorption capacities
properties, such as swel ing, solubility, alkaline water

retention, water and oil absorption, gelation and pasting
The method of Beuchat (1977) was employ and to determine the oil
characteristics.
and water absorption capacities of the starch.




Gelation studies
MATERIALS AND METHODS


The gelation properties of the starch were determined as described
Sample
by Sathe and Salunkhe (1981a).


Red sorghum grains were col ected from Institute of Agriculture

Research, Samaru, Zaria, Nigeria. The grains were cleaned and
Alkaline water retention
freed of mold or weathering. Al chemicals were reagent grade.


1.0 g of each sample was quantitatively transferred into a test tube

and weighed (w
Starch isolation
1). 5.0 ml of 0.1 M NaHCO3 was added and mixed
for 30 s (Fisher Vortex Genie 2TM Mixers). The sample was then

al owed to stand at 30±2°C for 20 min, centrifuged (200 rpm, 15
The method of Watson et al. (1955) was employed, with
min) and drained for 10 min at an angle 10–15° to the horizontal.
modifications, for the starch isolation.
Test tube with the content was then weighed (w

2) and the alkaline
water retention calculated as fol ows alkaline water retention

capacity (g/g) of sample w
Modifications of red sorghum starch
2 – w1.



Heat-moisture treatment: HMT was carried out using the method
Rapid visco analysis measurement
of France et al. (1995). The moisture levels of the starch samples

were increased to 18, 21, 24, and 27% by adding the appropriate
The paste viscosity of red sorghum starch was evaluated by RVA.
amount of distil ed water. The mixtures were stirred; the sealed
In the RVA, the short temperature profile (13 min) was used and the
samples in glass jars were heated in an air oven at 100°C for 16 h.
mixture was stirred at 960 rpm for l0 s and then at 160 rpm for the
After cooling, the jars were opened and the starch samples were air
remainder of the test. A mixture of 3.5 g starch and 25.0 ml water
dried to a moisture content of 10%.
was held at 50°C for 1 min and subsequently, heated to 95° at

12.2°C/min.
Annealing: The method of Knutson (1990) was adopted in
Holding time at 95°C was 2.5 min, subsequently the sample was
preparation of annealed red sorghum starch. The starch was
cooled to 50°C at 1.2°C/min, where it was kept for 2.1 min.
annealed by heating 100 g of starch in excess water at a
temperature of 50°C slightly above gelatinization temperature for 24

h Sample was centrifuged to remove excess water and air-dried.


RESULTS AND DISCUSSION


Effect of temperature on solubility and swelling
The effect of temperature on swel ing power of red

sorghum starch (Table 1) revealed that each type of
A starch sample 1.0 g was accurately weighed and quantitatively
transferred into a clear dried test tube and re-weighed (w
starch swel s differently, indicating differences in the
1). The

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930 Afr. J. Biotechnol.



Table 1. Effect of temperature on swel ing of native and modified red sorghum starches.

Swelling Power
RNS (%)
RSAN (%)
RHMT18
RHMT21
RHMT24
RHMT27
60°C
3.24±0.04 1.72±0.03
2.96±0.03
3.24±0.02
2.29±0.02
3.34±0.02
70°C
4.94±002
5.92±0.02
4.13±0.03
4.63±0.03
3.74±0.04
3.93±0.03
80°C
6.60±0.04 7.32±0.02
6.23±0.03
6.60±0.02
6.61±0.02
5.20±0.01
90°C
9.93±003
9.24±0.04
7.85±0.03
7.10±0.01
7.46±0.02
5.91±0.02

Al values are means of triplicate determination ± S.D.
RNS: Red sorghum native starch.
RSAN: Red sorghum annealed starch.
RHMT18-27: Red sorghum heat moisture treated starches.


Table 2. Effect of temperature on solubility of native and modified red sorghum starches.

Swelling Power
RNS (%)
RSAN (%)
RHMT18
RHMT21
RHMT24
RHMT27
60°C
1.98±0.04
0.64±0.02
0.14±0.01
0.46±0.02
0.83±0.03
0.50±0.02
70°C
2.08±002
0.70±0.01
0.61±0.03
0.70±0.01
1.34±0.02
0.60±0.01
80°C
2.34±0.03
1.90±0.04
1.03±0.03
1.21±0.04
2.06±0.02
1.54±0.04
90°C
3.03±003
4.20±0.02
2.24±0.04
3.24±0.02
3.25±0.02
4.41±0.07

Al values are means of triplicate determination ± S.D.
RNS: Red sorghum native starch.
RSAN: Red sorghum annealed starch.
RHMT18-27: Red sorghum heat moisture treated starches.


Table 3. The effect of ph on the swel ing power of red sorghum starches (native and modified).

pH
RNS (%)
RSAN (%)
RHMT18
RHMT21
RHMT24
RHMT27
2
2.6±0.4
0.72±0.07
0.53±0.06
0.38±0.07
0.34±0.06
0.21±0.06
4
3.2±0.4
0.28±0.06
0.43±0.05
0.47±0.06
0.37±0.06
0.23±0.04
6
3.5±0.6
0.41±0.06
0.37±0.06
0.44±0.05
0.43±0.06
0.36±0.08
8
4.0±0.6
0.44±0.04
0.42±0.06
0.53±0.05
0.43±0.06
0.46±0.05
10
5.6±0.6
0.47±0.04
0.48±0.06
0.60±0.07
0.49±0.06
0.53±0.05
12
7.8±0.6
0.48±0.06
0.65±0.06
0.61±0.06
0.51±0.07
0.55±0.07

Al values are means of triplicate determination ± S.D.
RNS: Red sorghum native starch.
RSAN: Red sorghum annealed starch.
RHMT18-27: Red sorghum heat moisture treated starches.


molecular organization within the granules. However, the
solubility. This is probably due to the weathering of the
swel ing power of starch increased with temperature. The
starch granules during HMT leading to improved solubility
degree of swel ing and the amount soluble components
(Shieldneck and Smith, 1971). HMT al owed the amylose
depends on the starch species (Schoch, 1964). There
molecules located in the bulk amorphous regions to
was a decrease in swel ing power and solubility of the
interact with the branched segments of amylopectin in the
annealed starch compared to the native starch due to the
crystal ine regions (Hoover et al., 1993; Hoover and
ordering rearrangement of starch molecules in the
Manuel, 1994).
granules. Eerlingen et al. (1997) proposed that the
The effect of pH on the swel ing power of red sorghum
decrease in swel ing powers and the increase in
starches (Table 3) showed that increase in pH leads to
gelatinization temperature were caused by transformation
increase in the swel ing power for al starches in the
of amorphous amylose into a helical form, increase in
alkaline region (pH 8–12) while there were very little
interactions between amylose chains, and alteration in
increase in the acidic region (pH 2–6). Shieldneck and
the interaction between crystal ites and the amorphous
Smith (1971) reported similar findings at alkaline pH.
matrix during annealing.
Native starch exhibited a higher solubility than the
The solubility of al the starches increased with
modified starches (Table 4). RSAN exhibited a maximum
temperature (Table 2). HMT27 showed the highest
at pH 2, which indicated good applications in acidic food

---

Adebowale et al. 931



Table 4. Effect of pH on solubility of native and modified red sorghum starches.

pH
RNS (%)
RSAN (%)
RHMT18
RHMT21
RHMT24
RHMT27
2
3.4±0.6
0.71±0.07
0.11±0.05
0.23±0.05
0.38±0.07
0.25±0.05
4
2.2±0.5
0.46±0.05
0.18±0.05
0.04±0.03
0.44±0.05
0.38±0.05
6
4.6±0.6
0.42±0.06
0.63±0.07
0.17±0.05
0.53±0.06
0.41±0.05
8
7.3±0.6
0.28±0.06
0.45±0.04
0.41±0.05
0.35±0.05
0.39±0.06
10
10.2±0.5
0.41±0.06
0.40±0.05
0.27±0.05
0.39±0.07
0.48±0.06
12
12.2±0.6
0.47±0.07
0.98±0.05
1.34±0.06
0.50±0.05
0.53±0.05

Al values are means of triplicate determination ± S.D.
RNS: Red sorghum native starch.
RSAN: Red sorghum annealed starch.
RHMT18-27: Red sorghum heat moisture treated starches.



Table 5. Gelation capacity of native and modified red sorghum starches.

Sample
Native RNS
Annealed RSAN
HMTR18
HMTR21
HMTR24
HMTR27
concentration
3
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
6
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
9
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
12
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
? Viscous
15
+ Gel
+ Gel
? Viscous
? Viscous
? Viscous
? Viscous
18
+ Gel
+ Gel
+ Gel
? Viscous
+ Gel
+ Gel
21
Firmgel
Firmgel
+ Gel
+ Gel
+ Gel
+ Firmgel
LGC
15
15
18
21
18
18

Determinations carried out in triplicates.
(?) No gelation, (+) gelation
LGC – Least gelation concentration.





Water and oil absorption capacities of the native and
WAC
OAC
modified are presented in Figure 1. Heat moisture
treatment linearly increased water binding capacity of
500
these starches, which implies that hydrophilic tendency
450
increased with increasing level of moisture treatment.
400
While there were decreases in oil absorption capacity
350
from 160mg/g in native starch to 150 g/g in RHMT27. This
300
result compared favourably with those obtained by Kulp
250
and Lorenz (1981) for potato and wheat starches.
200
Annealed starch here increased in water absorption
150
capacity indicating that the amorphous region may

A
b
s
o
r
p
t
i
o
n

(
g
/
g
)
100
%
expand slightly and some hydrogen bonds between the
amorphous and crystal ine regions could be broken.
50
There was increase in oil binding capacity, which shows
0
RNS
RSAN
RHMT
RHMT
RHMT
18
21
RHMT
24
27

the lipophilic nature of the outer covering formed in the

granule surface during annealing (Morrison et al., 1993).
Figure 1. Oil and water absorption capacities of native and
As the starch granules swel to form a gel by heating in
modified red sorghum starches. RNS, red sorghum native starch;
water, the amorphous region became hydrated. Table 5
RSAN, red sorghum annealed starch; RHMT18-27, red sorghum heat
moisture treated starches.
shows the effect of concentration on the gelation capacity

of the native and modified starches. Native starch did not

form a gel until it reached 15% concentration. Annealed
items. The increased solubility at alkaline pH may be due
starch had the same least gelation with the native starch
to increase hydrophilic characters of the starch at these
while the heat moisture treated starches from HMTR18,
pH values.
HMTR24 and HMTR27 had higher concentration than

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932 Afr. J. Biotechnol.



Table 6. Pasting properties of native and modified red sorghum starches.

Parameters
RNS Native Annealed RSAN
HMR18
HMR21
HMR24
HMR27
Peak Viscosity
97.00
365.04
257.08
172.08
119.67
126.78
Hot Pasting Viscosity
44.67
208.07
170.75
61.83
42.75
46.35
Breakdown
52.33
150.04
86.33
110.17
75.92
82.15
Final Viscosity
59.50
167.08
207.08
95.58
59.25
60.12
Set Back
14.83
126.19
36.33
36.75
16.50
18.56
Pasting Temperature
63.75
64.55
64.70
65.20
64.20
64.05

RNS: Red sorghum native starch.
RSAN: Red sorghum annealed starch.
RHMT18-27: Red sorghum heat moisture treated starches.




1.3
considerable increase in final viscosity from RSAN
1.2
HMTR18–HMTR21, which indicated dissolved starch
1.1
molecules into larger units as the solutions were cooled.
1.0
Annealed starch had the highest set back value, because
0.9
the tendency toward set back or gel formation has been
a
p
a
c
i
t
y

(
g
/
g
)
0.8
minimized in the heat-moisture treated starches.
0.7
According to Jacobs et al. (1995), both the formation of a
0.6
tightly packed array of swol en and deformable granules
0.5
and the leaching of amylose can contribute to viscosity
0.4
a
t
e
r

r
e
t
e
n
t
i
o
n

C
development in starch paste during heating and rigidity of
0.3
granule increases due to insufficient gelatinization. This
0.2
should give higher viscosity to paste because the rigid
0.1
A
l
k
a
l
i
n
e

w
granules are more resistant to shearing. The clarity of a
0.0
RNS
RSAN
HMTR
HMTR
HMTR
HMTR
18
21
24
27
starch gel directly influences the slime and colours of


products that contain it as a thickner. Annealed starch
Figure 2. Alkaline water retention of native and
had the highest breakdown compared with native starch
modified red sorghum starches. RNS, red sorghum
and heat-moisture treated starches indicating that it had
native starch; RSAN, red sorghum annealed starch;
less stability during heating, whereas peak viscosity
RHMT18-27, red sorghum heat moisture treated
increased after HMT.
starches.
In conclusion, starch obtained from red sorghum grains

can be modified physical y by two common modifications

such as annealing and HMT. Temperature exerted a
native starch. HMTR21 has the highest gelation capacity
change on the swel ing capacity and solubility of the
and it might be due to the increased quantity of the
starch, and also the starches behaved differently towards
amorphous phase, induced by transformation of the inter-
acidic and alkaline regions. Both annealing and HMT
crystal ine and crystal ine regions by HMT might cause an
increased the surface hardness of red sorghum starch
increased readiness of the structural transformation (Lim
gels and the hardness was inversely proportional to the
et al., 2001).
swel ing power. Therefore physical modifications would
Al the modified starches showed increase in alkaline
enhance gel formation, which is good for the food
water retention compared to the native starch (Figure 2).
industries.
This increase in water retention was attributed to the

surface area of the starch phase (Yamazaki et al., 1997).

The peak viscosity (pv) at any concentration is an
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