Sorghum Properties

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UUPhysicochemical Properties of Sorghum (Sorghum Bicolor L. Moench)

Starch as Affected by Drying Temperature
N. A. Aviara1*, J. C. Igbeka2 and L. M. Nwokocha3
1
Department of Agricultural and Environmental Resources Engineering,
University of Maiduguri, Maiduguri, Nigeria
2
Department of Agricultural and Environmental Engineering,
University of Ibadan, Ibadan, Nigeria
3
Department of Chemistry, University of Ibadan, Ibadan, Nigeria
*Corresponding author's e-mail:[email protected]
ABSTRACT
Starch was isolated from white sorghum grains and its proximate composition determined.
Scanning electron micrograph and x-ray diffraction pattern of the starch were obtained. The
effect of drying temperature in a tray dryer on physicochemical and pasting properties of isolated
starch was investigated.
The open air dried starch had a composition of 10.73% moisture, 0.30% ash, 1.06% protein and
1.07% fat. Amylose content was 21.08% and the average granule size and pH were 18.59μm and
5.45, respectively. The starch exhibited the A-type crystalline diffraction pattern, which was not
altered by drying in a tray dryer at the temperature range of 40 to 60oC. Water binding capacity
and swelling power of the open air dried starch were not significantly different from those of
starch dried at 40oC (p<0.05). Water binding capacity increased from 79.63 to 88.5%, while
swelling power, solubility and percentage of syneresis decreased from 12.01 to 8.96g/g, 7.08 to
2.85% and 14.00 to 10.80%, respectively as the drying temperature increased from 40 to 60oC.
Paste clarity was low (22.50 – 26.20%) but increased with increase in drying temperature up to
50oC and decreased with further increase in temperature. Pasting properties of open air dried
starch differed significantly from those of starch dried at different temperatures. Peak viscosity
decreased from 398.75 to 325.25 RVU as the drying temperature increased from 40 to 60oC.
Setback viscosity increased with increase in drying temperature up to a point and decreased with
further increase in temperature. Final and breakdown viscosities as well as pasting temperature
and peak time had polynomial relationships of the third order with drying temperature.
Regression equations that could be used to adequately express the relationships existing between
the physicochemical and pasting properties of sorghum starch and drying temperature were
established. These models could be used to select the drying temperature that would yield starch
of desired physicochemical properties for a functional application.
Keywords: White sorghum starch, degree of crystallinity, physicochemical properties, pasting

properties, drying temperature, tray dryer.
N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

(Sorghum Bicolor L. Moench) Starch as Affected by Drying Temperature”. Agricultural
Engineering International: the CIGR Ejournal. Manuscript Vol. XII. May, 2010.
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1. INTRODUCTION
Sorghum (Sorgum bicolor L. Moench) belongs to the Gramineae family of crops and the
Andropogoneae tribe. The species sorghum bicolor L. Moench is cultivated throughout the
intertropical zone of Africa. In Nigeria, it is mainly grown in the region lying between the middle
belt and semi-arid zones. Sorghum grain has a high starch content of 60 – 80% (McNell et al.,
1975). Sorghum starch finds uses in the food, chemical, pharmaceutical and textile industries. As
a result of this, interest in sorghum starch has recently been on the increase (Elkhalifa et al.,
2004). The starch is normally isolated in aqueous medium and dried, packaged and supplied in
granular form. This made drying a fundamental unit operation in starch processing. Due to the
physical and chemical properties of starch, it is sensitive to heat when moist. Therefore, it
requires that drying should be carried out under conditions that will not affect the functionality.
The functionality of a starch type in a given application and therefore, its quality is determined
principally by the physicochemical properties and these properties include water binding
capacity, gelatinization temperature, swelling power and solubility, freeze-thaw stability, paste
clarity, paste viscosity, retrogradation and gel strength (Adebowale and Lawal, 2002). Elkhalifa
et al. (2004) noted that fermentation of sorghum flour increased the solubility of its starch,
decreased the water binding capacity and had no effect on the freeze-thaw stability and paste
clarity. Adebowale et al. (2005) reported that heat moisture treatment and annealing of red
sorghum starch increased the water binding capacity and pasting temperature but decreased the
swelling power and solubility. According to Zweifel et al. (2003), the drying conditions are
determinants for the phase morphology and structure of protein and starch in cooked pasta,
which in turn, governs the textural properties of the pasta. Odigboh and Mohsenin (1975)
reported that the drying temperature of isolated starch significantly decreased the paste viscosity
of native cassava starch and this was confirmed by the findings of Aviara et al. (2010). Swelling
power, solubility and gelatinization temperature of corn starch were reported to have been
affected by drying conditions (Haros and Suarez, 1997) and starches isolated from low and high
temperature dried pasta were found to exhibit lower peak viscosity than those from ultra high
temperature dried pasta (Yue et al., 1999). Wang et al. (2001) reported that the peak viscosity of
rice flour increased with increase in drying temperature, while the effect of drying temperature
on the starch properties was not evident.
In order to establish and control the drying conditions to yield starch with physicochemical
property values needed for a particular application, there is the need to determine the response of
these properties to starch drying temperature. Information on the effect of drying temperature on
the physicochemical properties of sorghum starch appears to be scanty; therefore, this study was
undertaken to investigate the changes in these properties of the starch due to drying temperature.
The properties studied include water binding capacity, swelling power and solubility, freeze-
thaw stability, paste clarity and pasting properties.

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2. MATERIALS AND METHODS
2.1 Isolation of sorghum starch

The grains of white sorghum from which starch was isolated were supplied from Kano and
procured from an outlet in Ibadan, Nigeria.
The grains were cleaned and soaked in warm water at the temperature of 35oC for 6h (Aviara,
2010) to loosen the starch granules from the protein matrix and inhibit microbial activity. The
soaked grains were washed and crushed in a disc attrition milling machine (wet milling) and the
paste obtained was mixed with sufficient amount of water to form slurry. The slurry was sieved
through a muslin cloth and 75μm mesh size sieve. The residue was thoroughly washed and
discarded, and the starch milk collected was washed several times in aqueous alkaline medium to
remove the encapsulating protein matrix and allow the starch to settle. The supernatant was
decanted and the starch milk obtained was washed several times with decanting of water to
remove impurities and protein residue. The sorghum starch obtained was divided into two
portions and utilized in further investigations.
The first portion was dried in open air and used for proximate composition and pH determination
and scanning electron microscopy. The second portion was used to obtain starches dried in thin
layer in a tray dryer at the temperatures of 40, 50, 55 and 60oC respectively. The x-ray diffraction
pattern and physicochemical properties of the open air dried starch and those dried at different
temperatures were determined.
2.2 Determination of proximate composition

The moisture content of starch was determined by weighing using the AACC standard method,
(AACC, 2000). Five grams of open air dried starch was weighed in triplicate into previously
dried and weighed crucibles. These were placed in an oven and dried at 105oC to constant weight.
The crucibles and contents were allowed to cool in a dessicator and weighed. The moisture
content was calculated as percentage loss in starch weight reported to dry basis.
The ash content was determined using 2g of the starch samples used in moisture content
determination. This was ashed in a muffle furnace at 650oC until a constant weight of ash was
obtained. The ash content was calculated as weight of ash obtained per weight of starch (dry
basis) expressed in percentage. This was repeated three times and the average value was
determined.
The crude protein content was determined using 1.5g of starch weighed into a Kjeldahl long neck
digestion flask. 10ml of concentrated H2SO4 was added and the mixture swirled to wet the starch.
A piece of Kjeldahl tablet was added and the sample was digested over a heating mantle with
occasional swirling until a clean clear solution was obtained. Heating was continued for 30 mins
after which the flask and its content was allowed to cool. The content of the flask was transferred
into a 500ml Quickfit distillation flask. The Kjeldahl flask was filled to 2/3 of its volume with
distilled water, rinsed thoroughly and the water transferred into the Quikfit distillation flask. The
rinsing and transferring of water was repeated and the volume made up to 250ml. Some pieces of
zinc granules were added and 70 ml of 40% NaOH solution was ran down continuously by the
side into the flask. The distillation equipment was assembled with a delivery adaptor dipping into
25ml of 2% boric acid solution containing three drops of screened methyl red indicator. It was

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noted that during the distillation process, the green color of boric acid indicator and indicator
mixture turned pink. The ammonia liberated into the boric acid solution was titrated with
standard hydrochloric acid until the pink color turned purple.
The protein content of starch was determined using the following equation:
Percentage protein =
V  N  1.4  F 
W  % DM
(1)
where
V = volume of HCl used (ml)
N = molarity of the HCl solution
F = conversion factor from Nitrogen to protein: 6.25
W = weight of starch used (g)
%DM = percentage of dry matter
A blank determination of protein content following the above procedure without starch sample
was also carried out.
The crude fiber content was obtained using 2g of starch sample weighed into a 500ml conical
flask and 100ml of digestion reagent added. This was boiled on an electric heater and allowed to
simmer under reflux for 40 mins with the content of the flask swirled from time to time to ensure
an even digestion. The flask was removed and cooled under a cold water tap. The content was
filtered through a Whatman No.4 filter paper and washed several times with hot water. The paper
was opened and the residue transferred into a porcelain dish. This was dried for 2 h at 100oC,
cooled for 3 mins in a desiccator, weighed and ashed in a muffle furnace at 600oC for 30 mins.
The residue was cooled in a desiccator and reweighed. The crude fiber content of starch was
taken as the loss in weight on ashing, expressed as a percentage of the starch sample weight.
The fat content of the starch was determined by carrying out the ether extraction using a soxhlet
extractor.
The amylose content of starch was determined using the method of IITA (1995). 100mg of starch
sample (db) was weighed into boiling tubes. 1ml of ethanol (95%) was added and the mixture
swirled. 9ml of 1M NaOH solution was then added. The tubes and their contents were heated in
boiling water bath for 10 minutes to gelatinize the starch. The tubes were removed, cooled and
their contents transferred into 100ml standard volumetric flask. The volume was made up to
mark with distilled water and the flask shaken thoroughly and allowed to stand. 2.5ml of the
gelatinized starch solution was poured into a 50ml volumetric flask and 0.5ml of 1M acetic acid
added to acidify the solution. 1ml of iodine solution was then added. The flask was shaken and
left for 20 minutes for color to fully develop. The absorbance of the solution was monitored
using a SpectrumLab 752S uv visible spectrophotometer at 620 nm. Iodine solution of the same
concentration as that used in color development was used with distilled water in the reference
cell.
Amylose content = (% amylose of standard x absorbance of sample)

(2)
absorbance of standard

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2.3 Starch pH
2g of starch (db) was dispersed in 20ml of distilled water in long neck 50ml beaker for 1h at
room temperature. The pH was, thereafter, measured using a WPA CD70 pH meter. This was
replicated thrice and the average pH of the starch was determined.
2.4 Starch Microscopy

Granule micrographs were obtained using a JSM 35 Genie Scanning Electron Microscope (SEM).
The starch was sprinkled onto a double-backed adhesive carbon tab stuck to a circular aluminium
stub. The aluminium stub with the starch sample on it was placed in the vacuum chamber of a
polaron PS3 sputter coater. After attaining a vacuum of 0.1 to 0.2 torr and plasma current of 42
mA, the gold coating process was carried out for 140s. The stub with gold coated starch was then
placed in the SEM chamber which was evacuated before the electron beam was turned on. A
10kV, 2.05A setting was used for the subsequent imaging work on starch, the aperture size being
fixed at 3. Granule size was then analyzed using a BT1600 Image Analyzer.
2.5 Thin layer drying of starch

The initial moisture content of the starch used in carrying out thin layer drying was determined in
triplicate and the average value was recorded. The drying equipment used was a Laboratory
model tray dryer fitted with a temperature control device. It consisted of a drying chamber in
which perforated trays were arranged vertically and placed horizontally, a plenum chamber
where the heating elements were installed, a 0.374kW axial flow fan that supplied the drying air
at a rate of 0.238 m3/s and an outlet for discharging the used air.
Air at the ambient condition of 27 to 38oC dry bulb temperature, 23 to 26oC dew point
temperature and 50 to 78% relative humidity, was heated to the drying temperatures of 40, 50, 55
and 60oC respectively. For an experimental run at each drying temperature, the fan was turned on
and the dryer allowed running empty for 2 h to enable it to stabilize at the specified air condition
before the test began. 25g of starch at the initial moisture content was weighed in triplicate into
drying dishes and placed on the drying trays in the drying chamber with the fan running. Change
in sample weight was monitored by weighing periodically using an electronic balance. Weighing
of samples was carried out as follows, every 10 minutes for the first 1h; every 30 minutes for the
next 3h; every 1h for the next 3h; every 2h for the next 6h. Weighing was continued until three
consecutive readings gave identical weights. The test was then terminated and equilibrium with
the drying environment was assumed to have been reached. The moisture content of the samples
was determined at this point and taken to be the dynamic equilibrium moisture content. The
average dynamic equilibrium moisture contents of the starch at the different drying temperatures
were recorded.
2.6 X-ray diffraction

X-ray diffraction measurements were carried out on samples of open air dried starch and those
dried in thin layer in a tray dryer at different temperatures, using an MD10 2.04 diffractometer
that produced a monochromatic CuKα radiation (wave length = 1.54Ǻ, voltage = 25kV, current
400μA and exposure time = 1200s).

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The x-ray diffraction patterns of open air and tray dryer dried starches were used to classify the
sorghum starch and compute the degree of crystallinity. The degree of crystallinity of the starch
samples was determined using the method reported by Wang et al. (2005). This involved the
connection of the peak baselines of the diffraction pattern with a smooth curve. The upper
diffraction peak area and the total area over the diffraction angle, 2θ of 5 to 30o were graphically
determined and the ratio of the upper area to the total diffraction pattern area was taken as the
degree of crystallinity and expressed as follows.
Ac
Crystallinity,% 
 Ac  Aa 
(3)
where
Ac = area of the crystalline region of the X-ray diffractogram
Aa = area of the amorphous region of the X-ray diffractogram.
2.7 Physicochemical and pasting properties

The physicochemical properties of open air dried starch and those dried in a tray dryer at
different temperatures were determined in triplicate as follows:
Water binding capacity was determined using the method of Medcalf and Gilles (1965) as
reported by Nwokocha (2002). 2g of starch was weighed into a centrifuge tube and 25ml of
distilled water was added. The tube was corked and agitated on a shaker for 1h at room
temperature. It was then removed and centrifuged at 6000 rpm for 10 minutes. The water
released was decanted and the tube drained at a tilt angle of 45o for 5 minutes. The tube was
weighed and the amount of bound water was determined. The water binding capacity was
expressed as percentage of bound water to starch by weight (db).
Swelling power and solubility of starch was determined using the method of Konik et al. (1993).
About 0.5g of starch was weighed into centrifuge tube and 25ml of distilled water added. This
was immersed in a water bath at the temperature of 85oC for 30 minutes. The slurry was stirred
thoroughly with glass rod throughout the period of heating. The tube was removed and cooled to
room temperature and then centrifuged at 6000 rpm for 15 minutes. The supernatant was
carefully sucked into a weighed crucible, weighed and evaporated over a steam bath and dried in
an oven at 120oC for 4 h. The paste was weighed and the swelling power calculated as weight of
sedimented paste per gram of starch (db). The difference in weight after drying the supernatant
gave the weight of the soluble components. Percentage solubility was calculated as weight of
soluble components per weight of starch (db).
The method of Singhal and Kulkarni (1990) was followed in determining the freeze – thaw
stability of starch. 0.5g of starch (db) in 10ml of distilled water in test tube was heated at 95oC
for 30 minutes with constant stirring. This was then removed, cooled with continuous stirring,
transferred into a weighed centrifuge tube and subjected to freezing for 18 h and thawing for 3 h.
It was then centrifuged at 6000 rpm for 10 minutes and the percentage of water separated to the
weight of paste was taken as a measure of the freeze – thaw stability.
Paste clarity was determined using the method of Singhal and Kulkarni (1990). This involved the
measurement of light transmitted by starch of a known concentration at 660 nm using a uv

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visible spectrophotometer. Starch paste was prepared by heating 0.2g of starch in 20ml of
distilled water in cap – sealed tubes in a water bath at 95oC (with occasional shaking to avoid the
formation of lumps) for 30 minutes. The light transmittance was determined with distilled water
used in the reference cell.
The pasting characteristics of starch were determined using a Rapid Visco Analyser (RVA)
Series 4, Newport Scientific Ltd, Sydney, Australia. 3g (db) of starch sample in 25ml of distilled
water was shaken well and poured into a canister. A paddle was placed inside the canister and
centrally positioned onto the paddle coupling and the set up was inserted into the RVA machine.
The measurement circle was initiated by actuating the instrument motor. The profile was
observed as it ran on the monitor of the computer that was connected to the instrument. The 12
minutes profile was used. The time – temperature regimes used were: idle (starting) temperature
of 50oC for 1 min, heating from 50oC to 95oC in 3 minutes, 45s, holding at 95oC for 2 minutes
30s, cooling back to 50oC over 3 minutes 45s and maintaining the 50oC for 2 minutes. The starch
pasting properties namely viscosity, final viscosity, setback viscosity, breakdown viscosity,
pasting temperature and peak time were obtained.
2.8 Statistical Analysis

The data obtained were subjected to one way Analysis of Variance (ANOVA), Duncan multiple
range test and regression analysis. The results were used to determine the effect of drying
temperature on the physicochemical properties of sorghum starch and to establish the
relationship between starch properties and drying temperature treatment.
3. RESULTS AND DISCUSSION
3.1 Proximate composition

The proximate compostion and pH of the open air dried sorghum starch are presented in Table 1.
The moisture content was found to be 10.73 ± 0.211% and within the range of 10 – 20% for
commercial native starches (Soni et al., 1993). The ash content (0.30 ± 0.011%) was lower than
that of sweetsop and soursop starches (Nwokocha and Williams, 2009), higher than that of
treculia africana starch (Nwokocha and Ogunmola, 2005) and cocoyam starch and within the
same value as that of cassava starch (Nwokocha et al., 2009). The protein and fat contents of
1.06 ± 0.004% and 1.07 ± 0.001% respectively were higher than those of cassava starch
(Ogunmola et al., 2001), but lower than those of maize starch (Soni et al., 1990. The amylose
content (21.08%) was within the range reported for the starches of different varieties of sorghum
(Carcea et al., 1992) but lower than the values reported by Chanapamokkhot and Thongngam
(2007) and Boudries et al. (2009). The crude fiber in starch was found to be insignificant and the
pH was 5.45.

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Table 1. Proximate composition and pH of open air dried sorghum starch

Parameter
Value
Moisture content, %
10.73±0.211
Ash, %
0.3±0.011
Crude fiber, %
NIL
Crude fat, %
1.07±0.001
Protein, %
1.061±0.004
Amylose content, %
21.08±0.01
pH
5.45±0.105
3.2 Scanning Electron Microscopy

The scanning electron micrographs of sorghum starch dried in open air (A) and in a tray dryer at
60oC (B) are presented in Figure 1. The starch granules are irregular in shape with smoothened
edges and have unimodal distribution. An examination of the micrographs A and B in Figure 1
shows that drying sorghum starch in the temperature range employed did not change the shape
and surface features of the granules.

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(A)
(B)

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Figure 1. Scanning Electron Micrographs (SEM) of sorghum starch, A: open air dried and B:
dried in a tray dryer at 60oC, 1600X
The granule size analysis of the starch dried in open air (mildest drying condition) and at 60oC in
a tray dryer (harshest drying condition) is presented in Table 2. The starch dried in open air has a
granule size range of 5.44 – 19.02μm, average granule diameter of 11.27µm, L/D of 1.18 and
roundness of 0.79, while the starch dried at 60oC was of 5.42 – 19.39μm granule size range,
11.62μm average granule diameter, L/D of 1.14 and roundness of 0.81. These values are within
the range reported by Jane et al. (1994) and Choi et al. (2004). The granule size distributions of
the starch dried in the two conditions stated above are presented in Figure 2. This figure shows
that the drying of starch at the higher temperature of 60oC influenced the granule size
distribution. This could be attributable to a possible on set of swelling that must have occurred
when the granules at the high initial moisture content were exposed to the high temperature,
which was quite close to starch gelatinization temperature. Copeland et al. (2009) noted that the
gelatinization temperature of starches generally lies between 60 and 80oC.
Table 2. Granule size analysis of sorghum starch dried in open air and at 60oC
Particle characteristics open air dried starch
starch dried at 60oC
Particle Number 122

125
Maximum diameter (µm) 19.02
19.39
Minimum diameter (µm) 5.44
5.42
Average diameter (µm) 11.27
11.62
Length/Diameter, L/D 1.18
1.14
Roundness 0.79
0.81

11
40
35
30
ANS S
Percentage distribution %
25 60
20
15
10
0
9
9
99
9
.9
.9
.9
.9
.9
.9
.9
0.
12
14
16
18
20
‐6
‐8
‐1
0‐
0‐
0‐
0‐
0‐
00
00
00
.0
.0
.0
.0
.0
5.
7.
9.
11
13
15
17
19
Granule size distribution (nm)
Figure 2. Granule size distribution of sorghum starch dried at different temperatures: ANSS –
open air dried starch, 60 – starch dried at 60oC
3.3 Starch drying

The initial moisture content of the starch was found to be 84.5% (db). The dynamic equilibrium
moisture content obtained at the end of drying decreased with increase in drying temperature and
had a value of 8.70, 7.60, 5.80 and 4.18% (db) for sorghum starch dried at 40, 50, 55 and 60oC,
respectively.
3.4 X-ray diffraction pattern
The X-ray diffraction patterns of sorghum starch presented in Figure 3 shows that the starch
exhibited the A-type crystalline diffraction with major peaks at 15o, 17o, 18o and 23o. This
diffraction pattern is typical of cereal starches (Manek et al., 2005) and in agreement with the
finding of Abd Allah et al. (1987). The same peaks were found for starches from sorghum
varieties grown in the Sahara of Algeria (Boudries et al., 2009) and Korean waxy sorghum starch
(Shin et al., 2004). The A-type crystalline pattern of the starch was not altered by drying
temperature. Khunae et al. (2007) reported that the heat moisture treatment of rice starch did not
alter its A-type diffraction pattern. An opposite observation was however made on slowly
digestible non-pasted granular sweet potato starch (Shin et al., 2005).

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The relative crystallinity of sorghum starch dried at different temperatures is presented in Table 3.
The physical and chemical properties of a starch type are strongly dependent on its degree of
crystallinity (Frost et al., 2009). Increase in starch drying temperature caused the degree of
crystallinity to decrease from 36.5% for open air dried starch to 23.03% for starch dried at 60oC.
This could be due to the occurrence of thermal modification and annealing of starch granules as
drying temperature increased, resulting in the destruction of native starch crystals. Frost et al.
(2009) noted that the extrusion of starch to form thermoplastic starch destroyed native crystals as
a result of the occurrence of starch modification.
NSSA
NSS40
NSS50
NSS60
Intensity
5 10 15 20 25 30
2 theta
Figure3. Xray diffraction pattern of native sorghum starch dried at different
temperatures: NSSA - dried in open air, NSS40 - dried at 40oC, NSS50 - dried at
50oC and NSS60 - dried at 60oC
Table 3. Relative crystallinity of sorghum starch dried at different temperatures

Drying temperature, oC
Degree of crystallinity, %
Open air
36.5
40
34.18
50

13
30.65
55
24.87
60
23.03
3.5 Physicochemical properties

The mean values of the physicochemical properties of sorghum starch dried at different
temperatures are presented in Table 4.
Table 4. Physicochemical properties of sorghum starch dried at different temperatures

Drying Water Swelling Solubility Syneresis Paste
temperature binding power g/g % % clarity %
o
C capacity %
Open air 79.19±0.17d 13.006±0.975a 8.022±0.045a 15.10±0.01a 16.10±0.00d
40 79.63±0.68cd 12.01±0.614ab 7.08±0.140b 14.00±0.112b 22.50±0.75c
50 80.21±0.08c 11.23±0.25bc 6.54±0.38c 11.70±0.038c 26.20±0.19a
55 83.87±0.23b 10.76±0. 76c 3.33±0.08d 11.67±0.16c 25.00±0.04b
60 88.50±0.42a 8.96±0.182d 2.85±0.108e 10.80±0.002d 24.60±0.13b
Numbers in column denoted by the same letter are not significantly different (p<0.05)
3.5.1 Water binding capacity

Water binding capacity is a measure of the strength of starch intergranular bond. Low water
binding capacity is attributable to tight association (Soni et al.,1990), while high water binding
capacity is indicative of a loose association of native starch polymers or low lipid content
(Nwokocha and Ogunmola, 2005).
The water binding capacity of open air dried sorghum starch (Table 4) was not significantly
different from that of starch dried at 40oC in a tray dryer (p<0.05). The water binding capacity of
the starch increased significantly with increase in drying temperature. This implies that the
hydrophilic tendency of the starch increased with increase in its drying temperature. This may be
due to the expansion of the amorphous region of the starch (Adebowale et al., 2005) with
increase in drying temperature, and as a result of the occurrence of modification in which some
hydrogen bonds between the amorphous and crystalline regions got broken and the starch was
opened up to water imbibition. Similar effect on starch water binding capacity has been reported
as due to heat moisture treatment of chestnut starch (Singh et al., 2009) and reheating of
retrograded rice starch using microwave autoclave and steam (Han et al., 2009).

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The increase of starch water binding capacity with increase in drying temperature was linear and
could be expressed with the following equation:
ω = 0.6623T + 47.953, R2 = 0.98

(4)
where
ω = water binding capacity, %; T = drying temperature, oC and R2 = coefficient of determination.
The water binding capacity of sorghum starch was found to be higher than that of cassava starch
(Ikegwu et al., 2009, Aviara et al., 2010).
3.5.2 Swelling power and solubility

Swelling power and solubility provide information on the nature of the associative forces within
starch granules (Soni et al., 1990; Ogunmola et al., 2001). When starch is pasted in excess water
system, the granules imbibe water through the amorphous regions in a reversible manner, and the
amount of water imbibed increases with temperature until a critical temperature is reached
(gelatinization temperature) at which the starch swells irreversibly with loss of crystalline order.
This irreversible swelling is accompanied by significant uptake of water resulting in granule
expansion and leaching of amylose into solution (Pomeranz, 1990).
The swelling power of open air dried sorghum starch was not significantly different from that of
the starch dried at 40oC (p<0.05), while the solubility of the open air dried starch was
significantly higher than that of starch dried at different temperatures. Increase in drying
temperature significantly decreased the solubility of the starch and beyond 50oC; it significantly
decreased the swelling power (Table 4). This could be due to the ordering rearrangement of
starch molecules in the granules (Chung et al., 2000), transformation of the amorphous amylose
into helical form, increase in interaction between amylose chains or between amylose and
amylopectin chains in the amorphous regions, and alteration in the interaction between
crystallites and the amorphous matrix (Eerlingen et al., 1997) resulting from increase in the
annealing effect of starch drying as drying temperature increased. Olayinka et al. (2008)
explained that the decrease in the swelling power and solubility of heat moisture treated sorghum
starch compared with that of the native starch may have been due to granular stability resulting
from unraveling of the double helices that might have been present in a crystalline array in the
native granule. Decrease in swelling power and solubility could also have been due to amylose-
lipid complexation (Olayinka et al., 2008, Copeland et al., 2009) as it has been shown that
amylose inhibits granule swelling under conditions where amylose-lipid complexes are likely to
be formed (Olayinka et al., 2008). Gomes et al. (2004) and Adebowale et al. (2005) similarly
reported that the annealing of cassava starch and heat moisture treatment and annealing of red
sorghum starch, respectively decreased starch swelling power and solubility.
The relationship existing between the starch swelling power, solubility and drying temperature
was found to be polynomial of the second order which can be expressed using the following
equations:
φ = -0.0092T2 + 0.7736T – 4.2615, R2 = 0.97

(5)

15
ς = -0.0156T2 + 1.3488T – 21.896, R2 = 1.00
(6)
where
φ = swelling power, g/g, ς = solubility, %.
The above relationships show that the solubility of sorghum starch increased with increase in it
swelling power. Soni et al. (1990), Soni et al. (1993) and Nwokocha and Ogunmola (2005) made
similar observations on the starches of quercus leucotrichophora (oak), cana edulis, maize and
treculia africana (African breadfruit) respectively, and attributed it to the fact that a part of the
linear component of the starch may have been involved in the micellar network, while the rest
was free from entanglement and therefore, was preferentially solubilized. The swelling power of
sorghum starch was higher than that of cassava starch, and the solubility of the starch dried at
temperatures below 50oC was higher than that of cassava starch (Ikegwu et al., 2009), while that
of the starch dried above 50oC was lower.
3.5.3 Freeze-thaw stability and paste clarity

Freezing a starch gel normally leads to the formation of ice crystals and the concentration of
starch in the non-ice phase. Upon thawing, the water is easily expressed from the network, giving
rise to the phenomenon known as syneresis. The ability of starch gel to withstand this
phenomenon during freeze-thaw cycling (freeze-thaw stability) enhances its potential use in
frozen food products (Baker and Rayas-Duarte, 1998). The level of syneresis is inversely
proportional to the freeze-thaw stability of a starch gel.
The freeze-thaw stability of open air dried sorghum starch (Table 4) was significantly different
from that of starch dried at different temperatures in a tray dryer (p<0.05). The freeze-thaw
stability of starch dried at 50 and 55oC respectively, as measured by the level of syneresis, was
not significantly different. Syneresis in the starch was however, found to decrease
logarithmically with increase in drying temperature. The relationship existing between
percentage of syneresis and drying temperature could be represented by the following equation:
τ = -7.648LnT + 42.066, R2 = 0.95

(7)
where
τ = percentage of syneresis, %.
This implies that freeze-thaw stability increased with increase in drying temperature and could
be attributed to changes in starch crystallinity due to partial crystallite melting, realignment of
polymer chains and possible enlargement of the amorphous regions of the starch, arising from
increase in drying temperature. Atichokudomchai et al., (2002) reported that the freeze-thaw
stability of acid-modified tapioca starch increased with annealing. Luo et al., (2006) noted that
the freeze-thaw stability of maize starch increased with microwave irradiation and attributed the
result to increase in the magnitude of hydrogen bonding forces (interaction between amylose-
amylose and amylose-amylopectin chains) within starch granules due to irradiation.
One of the major uses of starch is to impart viscosity to food, and the clarity of a starch paste is
one of its important attributes in this function. Starch used to thicken fruit pie filling is preferably
transparent, but starch used in spoonable salad dressing should be opaque. There are several

16
definitions that have been given to starch paste clarity. These include light transmittance
characteristics (Hoover and Hadziyev, 1981; Maningat, 1986), light reflectance characteristics
(Schoch, 1942) and degree of whiteness (Marrs et al., 1977) of starch paste.
The paste clarity of open air dried sorghum starch was significantly different from that of starch
dried at different temperatures in a tray dryer (p<0.05). The paste clarity of starch dried at 55 and
60oC was not significantly different. Paste clarity increased with drying temperature up to a point
and decreased with further increase in temperature. It had a relationship with drying temperature
that was found to be polynomial of the second order and could be expressed with the following
equation:
ρ = -0.0235T2 + 2.4477T – 37.677, R2 = 0.95
(8)
where ρ = paste clarity, %.

This may be due to improvement of amylose leaching and enhancement of interactive bond
formation between amylopectin molecules with increase in drying temperature up to a point after
which granule remnants connected by a matrix of leached amylose and amylopectin increased
and caused decrease in paste clarity.
3.5.4 Pasting characteristics

The pasting properties of starch are used in assessing the suitability of its application as
functional ingredient in food and other industrial products. The most important pasting
characteristic of granular starch dispersion is its viscosity. High paste viscosity suggests
suitability as thickening agent in food (Rapaille and Vanhemelrijck, 1999) and as finishing agent
in textile and paper industries (Nwokocha, 2002).
The pasting properties of sorghum starch dried in thin layer in open air and in a tray dryer at
different temperatures are presented in Table 5. The pasting curves of the starch dried are
presented in Figure 4.
Table 5. RVA pasting properties of sorghum starch dried at different temperatures

Drying Peak viscosity Final Breakdown Setback Pasting Peak
temperature RVU viscosity viscosity RVU viscosity temperature time
o o
C RVU RVU C minutes
Open air 335.25 311.75 157.33 133.83 80.70 4.27
40 398.75 286.42 216.33 104 80.90 4.33
50 377.33 321.42 190.92 135 81.75 4.40
55 368.42 291.58 216.92 140.08 80.90 4.20
60 325.25 311.75 145.17 131.67 81.75 4.60

17
400
300
200
Viscosity RVU
Y - NSSA
100
0 Newport Scientific Pty Ltd
0 3 6 9 12 15
Time, minutes
A
A
400 B
C
300
Viscosity RVU
200
A - NSS40
B - NSS50
100
C - NSS55
D - NSS60
0 Newport Scientific Pty Ltd
0 3 6 9 12 15
Time, minutes
B
Figure 4. RVA pasting curves of native sorghum starch, A: NSSA - dried in open air and B:
NSS40 – dried at 40oC, NSS50 – dried at 50oC, NSS55 – dried at 55oC and NSS60 – dried at
60oC in a tray dryer

18
Table 5 shows that the peak viscosity of open air dried starch was lower than that of starch dried
at 40, 50 and 55oC but higher than that of starch dried at 60oC. The peak viscosity decreased with
increase in drying temperature in a relationship that was found to be polynomial of the second
order and could be expressed with the following equation:
υp =-0.2017T2 + 16.684T + 53.075, R2 = 0.96

(9)
where
υp = peak viscosity, RVU.
According to Jacobs et al. (1995), both the formation of a tightly packed array of swollen and
deformable granules and leaching of amylose can contribute to viscosity development in starch
pastes. Decrease in swelling power with increase in starch drying temperature was expected to
lead to increase in paste peak viscosity as a result of increase in the rigidity of granules (Chung et
al., 2000) due to insufficient gelatinization. The decrease in peak viscosity of sorghum starch
with increase in drying temperature could therefore be due to increase in the annealing effect of
heated air drying on the starch as the drying temperature increased. Gomes et al. (2004),
Olayinka et al. (2008) and Han et al. (2009) respectively noted that the annealing of cassava
starch, heat-moisture treatment of sorghum starch and autoclave reheating of retrograded rice
starch decreased the peak viscosity.
The peak viscosity of sorghum starch used in this study was lower than that of starches from
sorghum varieties grown in Zimbabwe (Beta et al., 2000) and Algeria (Boudries et al., 2009).
The final viscosity of open air dried sorghum starch was higher than that of starch dried at 40 and
55oC respectively, but did not differ from that of starch dried at 60oC and was lower than that of
starch dried at 50oC. The final viscosity increased with increase in drying temperature up to a
point indicating that dissolved starch molecules must have increasingly formed into larger units
(Adebowale et al., 2005) as drying temperature increased and the solution of starch was cooled.
Thereafter, the final viscosity decreased with further increase in temperature as a result of the
breakage of some hydrogen bonds within the starch granules. Chung et al. (2000) reported that
the final viscosity of mung bean starch gel increased with increase in annealing temperature and
thereafter, decreased with further increase in annealing temperature. The relationship existing
between final viscosity and starch drying temperature was found to be polynomial of the third
order which could be represented with the following equation:
υf = 0.0816T3 – 12.459T2 + 627.22T - 10089, R2 = 1.00

(10)
where
υf = final viscosity, RVU.

19
Breakdown viscosity is used in assessing the ability of a starch paste used as thickener to
withstand severe processing conditions. During breakdown, the starch macromolecules and
swollen granules undergo fragmentation resulting in lowering of viscosity. Pukkahuta et al.
(2007) and Pukkahuta and Varavinit (2007) reported that increase in the temperature of heat-
moisture and osmotic pressure treatments decreased the breakdown viscosity of starches. The
breakdown viscosity of open air dried sorghum starch was lower than that of the starch dried at
40, 50 and 55oC, but higher than that of starch dried at 60oC. Below 60oC, drying temperature
did not significantly affect the breakdown viscosity of the starch. This may have been caused by
the strengthening (stabilization) of the starch polymers through non-disruption of the hydrogen
bonds within the granules, thereby preventing the association of amylose molecules after cooling
(Gomes et al., 2004). The breakdown viscosity of the starch had a relationship with drying
temperature that was polynomial of the third order. This relationship could be expressed using
the equation
υb = -0.1236T3 + 18.431T2 – 907.68T + 14941, R2 = 1.00

(11)
where
υb = breakdown viscosity, RVU.
Setback viscosity is a measure of retrogradation, that is the extent to which dissolved starch
macromolecules – amylose – are able to reassociate with themselves and granule fragments.
During setback, the solubilized amylose molecules reassociate through the formation of a three
dimensional network which results in a gel. The setback viscosity of open air dried sorghum
starch was higher than that of starch dried at 40 and 60oC but lower than that of starch dried at 50
and 55oC. Setback viscosity increased with increase in drying temperature up to a point and
decreased with further increase in temperature. It was speculated that the initial increase in
setback could be due to disordered linear amylopectin chains (Tattiyakul et al., 2007) being
readily aligned with other adjacent linear branches to form gel with more widely spaced junction
zones in the network aggregates. Decrease in setback with further increase in drying temperature
may be due to the annealing effect drying at such temperature level resulting in starch
stabilization and preventing the association of amylose molecules (Gomes et al., 2004). Setback
viscosity varied with drying temperature according to a polynomial relationship of the second
order. This relationship could be represented by the following equation:
υs = -0.1806T2 + 19.476T – 386.32, R2 = 0.99

(12)
where
υs = setback viscosity, RVU.
The pasting temperature of open air dried sorghum starch was lower than that of starch dried at
different temperatures in a tray dryer. There was no significant difference between the pasting
temperatures of starch dried at 40 and 55oC and at 50 and 60oC, respectively. High pasting
temperature indicates that the starch molecules may have had more mobility and undergone
conformational reorganization (Petitot et al., 2009), and low pasting temperature suggests that

20
fewer associative forces and crosslinks were present within the starch granules (Olayinka et al.,
2008). A combination of these phenomena may have induced the non-significant variation of the
pasting temperature with drying temperature. The pasting temperature had a polynomial
relationship of the third order with drying temperature, which could be expressed with the
following equation:
Tp = 0.0025T3 - 0.3868T2 + 19.338T - 237, R2 = 1.00

(13)
where
Tp = pasting temperature, oC.
The peak time of open air dried sorghum starch was lower than that of starch dried at different
temperatures. Peak time did not significantly increase with drying temperature. Chung et al.
(2000) reported that the annealing of mung bean starch did not significantly change the peak
time. The relationship existing between the peak time of starch and drying temperature was
found to be polynomial of the third order. This relationship could be represented by the
following equation:
tp = 0.0008T3 – 0.1129T2 + 5.5478T - 84.45, R2 = 1.00

(14)
where
tp = peak time, minutes.
4. CONCLUSIONS
The results of this study show that the proximate composition of open air dried sorghum starch
was 10.73% moisture, 0.30% ash, 1.06% protein and 1.07% fat. The amylose content was
21.08% and the pH was 5.45. The granules were irregular in shape and it had unimodal
distribution. The average granule size was 11.27μm. Drying of starch at the higher temperature
of 60oC slightly increased the granule size. The starch exhibited the A-type crystalline diffraction
pattern which was not altered by drying temperature. The degree of crystallinity decreased with
increase in drying temperature.
Increase in drying temperature significantly (p<0.05) increased starch water binding capacity and
decreased the swelling power and solubility. Percentage of syneresis decreased implying that
freeze-thaw stability increased with increase in drying temperature. Paste clarity was low but
increased with increase in drying temperature up to 50oC and decreased with further increase in
temperature. Peak viscosity decreased as the drying temperature increased. Setback viscosity
increased with increase in drying temperature up to a point and decreased with further increase in
temperature and final and breakdown viscosities as well as pasting temperature and peak time
had polynomial relationships of the third order with drying temperature.
Regression models were used to express the relationships existing between the physicochemical
and pasting properties of the starch and drying temperature. These models could be used to select

21
the drying temperature that would yield starch with desired physicochemical properties for a
functional application.
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1

UUPhysicochemical Properties of Sorghum (Sorghum Bicolor L. Moench)

*Corresponding author's e-mail:[email protected]

Keywords: White sorghum starch, degree of crystallinity, physicochemical properties, pasting

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

2.1 Isolation of sorghum starch

2.2 Determination of proximate composition

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

Amylose content = (% amylose of standard x absorbance of sample)

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

2.4 Starch Microscopy

2.5 Thin layer drying of starch

2.6 X-ray diffraction

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

2.7 Physicochemical and pasting properties

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

2.8 Statistical Analysis

3. RESULTS AND DISCUSSION

3.1 Proximate composition

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

Table 1. Proximate composition and pH of open air dried sorghum starch

3.2 Scanning Electron Microscopy

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

starch dried at 60oC

Particle Number 122

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

3.3 Starch drying

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

Table 3. Relative crystallinity of sorghum starch dried at different temperatures

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

3.5 Physicochemical properties

Table 4. Physicochemical properties of sorghum starch dried at different temperatures

3.5.1 Water binding capacity

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

ω = 0.6623T + 47.953, R2 = 0.98

3.5.2 Swelling power and solubility

φ = -0.0092T2 + 0.7736T – 4.2615, R2 = 0.97

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

3.5.3 Freeze-thaw stability and paste clarity

τ = -7.648LnT + 42.066, R2 = 0.95

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

where ρ = paste clarity, %.

3.5.4 Pasting characteristics

Table 5. RVA pasting properties of sorghum starch dried at different temperatures

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

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0 Newport Scientific Pty Ltd

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

υp =-0.2017T2 + 16.684T + 53.075, R2 = 0.96

υf = 0.0816T3 – 12.459T2 + 627.22T - 10089, R2 = 1.00

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

υb = -0.1236T3 + 18.431T2 – 907.68T + 14941, R2 = 1.00

υs = -0.1806T2 + 19.476T – 386.32, R2 = 0.99

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

Tp = 0.0025T3 - 0.3868T2 + 19.338T - 237, R2 = 1.00

tp = 0.0008T3 – 0.1129T2 + 5.5478T - 84.45, R2 = 1.00

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum

N. A. Aviara, J. C. Igbeka and L. M. Nwokocha. “Physicochemical Properties of Sorghum