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Modification of Cassava Starch for Industrial Uses

Article  in  International Journal of Engineering and Technology · January 2012

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 International Journal of Engineering and Technology Volume 2 No. 6, June, 2012

Modification of Cassava Starch for Industrial Uses

Akpa, Jackson Gunorubon.1 and Dagde, Kenneth Kekpugile.2
Department of Chemical/Petrochemical Engineering
Rivers State University of Science and Technology,
Port-Harcourt, Rivers State, Nigeria

ABSTRACT
Cassava starch modification by cross-linking using four different reagents (ammonium phosphate, sodium acetate, sodium
acetate with adipic acid, sodium acetate with fumaric acid) was performed. Functional properties (ash content, pH, moisture
content, gelatinization temperature, swelling power, swelling volume, solubility and viscosity) of the modified starch were
compared with those of the native cassava starch. The modified starches had varying degrees of improvements in properties
in descending order as: modification with sodium acetate, ammonium phosphate, sodium acetate with adipic acid, sodium
acetate with fumaric acid. Starch modified with sodium acetate and ammonium phosphate showed great improvement in their
gelatinization temperature with values of 79oF and 75oF compared with 69oF of the native starch, solubility of 66.7% and
37.1% compared with 0% of the native cassava starch and had lower and stable viscosities.

Keywords: Cassava starch, modification, cross linking, functional properties

1. INTRODUCTION and storage particular at low pH. Native starches also

yield pastes of poor stability which decreases its shelf life
Starch is one of the most important but flexible food (storage stability) causes shrinkage and the release of
ingredients possessing value added attributes for water. In order to improve on the desirable functional
innumerable industrial applications. The most common properties and overcome its limitations, native starches
sources of food starch are corn, potato, wheat, are often modified. Modification, (alteration of the
cassava/tapioca and rice. Cassava is second only to sweet physical and chemical characteristics to improve
potato as the most important starchy root crop of the structural properties) can be used to improve inherent
tropics (Grace, 1977). It is now grown widely as food poor physio-chemical properties of native starch thus
crop and for industrial purposes. In Nigeria, cassava is a tailor it to specific industrial applications (Cock, 1982;
staple food for both rural and urban areas and in recent Miyazaki et al., 2006).
years it has been transformed from being a subsistent crop
to an industrial cash crop. Starch’s use now extends far Starch modification can be broadly grouped into four
beyond its original design as a source of biological classes namely: physical, chemical, enzymic and
energy. Practically every industry in existence uses starch biological modifications. Among these modification
or its derivatives in one form or another. In foods and methods, chemical means is the most frequently used
pharmaceuticals starch is used to influence or control such process (Daramola and Osanyinlusi, 2006). Chemical
characteristics as texture, moisture, consistency and shelf modification of starch involves the treatment of native
stability. It can be used to bind or to disintegrate; to starch with specific chemicals reagent. This definition
expand or to densify; to clarify or to opacify; to attract includes acetylated, oxidized, lintnerized,
moisture or to inhibit moisture; to produce smooth texture pyrodextrinized, hydroxypropylated and cross-linked
or pulpy texture, soft coatings or crisp coatings. It can be starches (Kaur et. al., 2004).
used to stabilize emulsions or to form oil resistant films.
Starch truly serves as a multifunctional ingredient in the Modification using the method of cross linking increases
food industry. (Miyazaki et al. 2006). the amylopectin content of native starch and makes the
starch more stable and particularly useful in adhesive
Native starches irrespective of their source are undesirable manufacture, paper making and used in frozen foods
for many industrial applications because of their inability (Hirsch and Kokini 2002). Cross-linking and substitution
to withstand processing conditions such as extreme are two methods for making modified starches. Cross-
temperature (has low thermal resistance), diverse pH and linked starch is more resistant to acid, heat and shearing
high shear rate (has low shear resistance) (Singh et al. than is native starch (Mirmoghtadaei, et al., 2009).
2007), high ability to retrograde, loss of viscosity, Therefore cross-linked starch is suitable for canned food,
syneresis tendency and thickening power upon cooking surgical dusting powder and other applications (Miyazaki
et al., 2006)
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 International Journal of Engineering and Technology (IJET) – Volume 2 No. 6, June, 2012

hydroxide mix thoroughly, add 6g of ammonium

In recent years, substantial progresses have been made in phosphate (cross linking agent) to the starch and mix
obtaining starches from non-conventional botanical thoroughly, dry in an oven and store in a plastic air tight
sources and studying their functional and container at room temperature.
physicochemical properties (Zhao and Whistler, 1994; Native cassava starch
Perez et al., 1997; Hoover, 2001; Nunez-Santiago et al.,
2004).
Add fluxing Agent
The objective of this study is to evaluate the effect of
modification by cross linking on some physicochemical Stir for 5 min
and rheological properties of starch obtained from a
species of Nigerian cassava (native starch). Starch
extracted from cassava is modify by the method of cross- Add Alkaline Catalyst
linking using ammonium phosphate, sodium acetate,
Mix for 20 min
sodium acetate with adipic and fumaric acids respectively
and its properties (gelatinization temperature, moisture Add cross linking agent
content, pH, viscosity, solubility, swelling power and
Neutralize with Acid
volume and ash content) determined and compared with
that of the unmodified native starch. These results may be Mix for 15 min
useful in finding new applications for this type of cross-
linked starch in food and non-food productions.

2. MATERIALS AND METHODS Heat in water bath maintained at 75OC

Freshly harvested cassava tubers (seventeen months old)

of specie TMS 55124 were obtained from the student’s Stir continuously for 1 hr, pour
demonstration farm of the Rivers State University of
out mixture to cool.
Science and Technology, Port Harcourt, Nigeria.
Figure 1: Flow chart for the preparation of modified cassava
2.1 Cassava Starch Preparation starch

Cassava starch was prepared following the method of 2.4 Preparation of Modified Starch With
Moorthy et al., (1999). Cassava roots were peeled, Sodium Acetate
washed and disintegrated in a grating machine. The
resulting cassava mesh was reground and mixed with Weigh 200g of native cassava starch into a plastic
water in the ratio 1:5 (w/v %). The mesh was filtered container, add 0.2g of silicon oxide (fluxing agent) to the
through double layer of nylon cloth to obtain starch starch, mix for 5 minutes, add 20g of sodium hydroxide
solution. The starch was separated from the water by (alkaline catalyst), mix for 20 minutes, add 29g of sodium
sedimentation and decantation. The starch was set in an acetate (cross linking agent) mix for 15 minutes, heat
oven to dry. The native starch was labelled 1. mixture in a water bath maintained at a temperature of
75°C, stir mixture continuously for 1hour, pour out the
2.2 Preparation of Modified Cassava mixture to cool.
Starches
2.5 Preparation of Modified Starch with
Four types of cross-linked cassava starches were produced Sodium Acetate and Fumaric Acid
as shown in Figure 1 using four different reagents:
ammonium phosphate, sodium acetate, sodium acetate Weigh 200g of native cassava starch into a plastic
neutralized with adipic acid and sodium acetate container, add 0.2g of silicon oxide, mix for 5 minutes,
neutralized with fumaric acid. The modified starches were add 20g of sodium hydroxide (alkaline catalyst), mix for
labelled 2, 3, 4 and 5 respectively. 20 minutes, add 29g of sodium acetate and 14.5g of
fumaric acid, mix for 15 minutes, heat mixture in a water
2.3 Preparation of Modified Starch with bath maintained at a temperature of 75°C, stir mixture
Ammonium Phosphate continuously for 1hour, pour out the mixture to cool.

Weigh 200g of native cassava starch into a plastic

container, add 2.4ml aqueous solution of sodium
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 International Journal of Engineering and Technology (IJET) – Volume 2 No. 6, June, 2012

2.6 Preparation of Modified Starch with minutes and weighed. 2g of each starch sample was put
Sodium Acetate and Adipic Acid into the dishes, weighed and labelled. The dishes were put
in an oven maintained at 105°C for 4 hours; the dishes
Weigh 200g of native cassava starch into a plastic were removed, placed in the dessicator and allowed to
container, add 0.2g of silicon oxide, mix for 5 minutes, cool for 15 minutes. The dishes were removed and
add 20g of sodium hydroxide (alkaline catalyst), mix for weighed as quickly as possible. The moisture content in
20 minutes, add 29g of sodium acetate and 14.5g of adipic the samples was calculated as follows:
acid, mix for 15 minutes, heat mixture in a water bath
maintained at a temperature of 75°C, stir mixture % Moisture = Weight moisture in sample x 100 (2)
continuously for 1hour, pour out the mixture to cool. Weight of sample before drying

3. CHEMICAL ANALYSIS 3.5 Determination of Swelling Volume,

Swelling Power and Solubility
After extraction and modification of the native starch,
The swelling power and solubility were determined in
some chemical tests were performed to determine thermal
accordance with the methods described by Hirsch and
and rheological properties of the starches and confirm any
KoKini, (2002). The samples were poured into graduated
improvements in quality of the modified starch when
centrifuge tubes appropriately labelled. The solution was
compared with those of the native starches; hence
ascertain the impact of modification. All results were the stirred, placed in a water bath heated to 95°C while
average of duplicate analysis. The ash content, pH, shaking the sample gently to ensure that the starch
gelatinization temperature, and moisture content were granules remain in suspension until gelatinization occurs.
determined according to the methods of Association of The gelatinized samples were held at 95°C in the water
Official Analytical Chemists (AOAC, 1984) bath for 1 hour. The samples were cooled to room
temperature under running water and centrifuged for 30
minutes at 1000rpm. After centrifuging, the swelling
3.1 Determination of Ash Content volume was obtained directly by reading the volume of
1.5g of sample was weighed into a crucible of known swollen sediment in the tube. The supernatant was
weight. The crucible was put into a furnace and the separated from the sediment, put in a metal dish, weighed,
sample left to ash. After ashing, the crucible was brought dried at 105°C for 1 hour, weighed and dried again. The
out of the furnace, cooled to room temperature and starch swelling power and solubility were determined
weighed. The ash content of the sample was calculated according to equations (3) and (4).
using the formula:
Swelling power = Weight of swollen sediment (3)
% ash in sample = Weight of ash in sample X 100 (1) Weight of dry starch
Weight of sample
Solubility = Weight of dry supernatant x 100 (4)
3.2 Determination of pH Weight of starch sample
This was determined using a pH meter (model HI 8424
3.6 Determination of Viscosity
with pH buffer 7). 1.5g of starch sample was dissolved in
beaker with 10ml of distilled water and stirred properly. The Viscosity profile of the native and modified starches
The pH meter was inserted into the solution and the was obtained using a viscometer (LvDv I+, Brookfield,
reading taken. USA) following the technique proposed by AOAC, 1884.
The gelatinized starch was heated to a desired temperature
3.3 Determination of Gelatinization and placed under the viscometer with the spindle
Temperature immersed in the beaker. The spindle was set at speeds rate
of 10, 20, 50, 100rpm and the viscometer readings taken
1.5g of starch sample was dissolved in a beaker with 10ml
at these speeds. This procedure is repeated for the all
of distilled water, mixture is stirred, a thermometer
starch samples at temperatures 10°C, 20°C, 30°C, 60°C
inserted and beaker placed in a water bath. The solution
was stirred continuously until its colour became milky and 80°C.
and thickened. This is the gel point and the temperature at
this point was read off as the gelatinization temperature. 4. RESULTS AND DISCUSSION
The results of the various analyses to determine the
3.4 Determination of Moisture Content thermal and rheological properties of the native and
Five clean metal dishes were dried in an oven for 15 modified starches such as the ash content, pH,
minutes at 105°C, allowed to cool in a dessicator for 10 gelatinization temperature, moisture content, swelling

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 International Journal of Engineering and Technology (IJET) – Volume 2 No. 6, June, 2012

volume, swelling power and solubility are presented in Table 1.

Table 1: Result of Quality Analysis of Starch Samples

Sample % Ash pH Gel. Temp. % Moisture Swelling Swelling Solubility

(OC) Volume Power (%)
1 0.153 5.41 69 12.50% 10.5 7.40 0
2 0.133 7.05 75 15.00% 4.5 3.76 37.06
3 0.123 7.54 79 11.75% 1.0 1.23 66.67
4 0.207 5.66 74 14.55% 4.5 3.57 39.40
5 0.033 7.13 77 13.50% 5.0 4.00 22.40

4.1 Ash Content native starch modified with sodium acetate with a
decrease. Mahmut and Sosulski (2004) and Huang et., al
The ash content of a sample is the non-volatile inorganic (2007) had earlier reported increased water absorption
matter of a compound which remains after subjecting it to ability of modified starches. Starch modified with
a high decomposition temperature. During heating, the ammonium phosphate and sodium acetate mixed with
organic compounds are decomposed or released leaving adipic acid had the highest moisture content of 15% and
behind the residue which consists mainly of other 14.55% respectively, the moisture content in the other
inorganic matters. Hence the ash content can be samples did not exceed the maximum allowable limit
considered an indication of clean processing.
Modification by cross-linking decreases the ash content of 4.4 Gelatinization Temperature
starch (Alejandro, et. al., 2008). This trend is obtained
from the results of the ash content of the modified The gelatinization temperature of starch is the temperature
starches shown in Table 1; indicating that modification by at which the starch forms a completely transparent gel.
cross-linking produces cleaner starches. However the Gelatinization is a process that breaks down the
neutralization of sodium acetate with adipic acid intermolecular bonds of starch molecules in the presence
increased the ash content. of water and heat and allows the starch molecules to
engage more water. This penetration of water increases
4.2 pH. randomness in the structure of the starch. As expected the
stronger the bond between the starch molecules, the
The pH of a substance is the degree of acidity or alkalinity higher the amount of heat required to break the inter-
of that substance. Starch pastes from cross-linked starches molecular bond and therefore, the higher the gel
have been reported to be less likely to break down with temperature (Singh-Sodhi and Singh, 2005). Cross-linking
extended cooking times and possess increased acidity or treatment is intended to add intra and inter-molecular
severe shear (Langan, 1986). Modification increased the bonds at random locations in the starch granule that
pH of the native starch from 5.41 to 5.66, 7.05, 7.13 and stabilize and strengthen the granule (Acquarone & Rao,
7.54 for modification with sodium acetate neutralized 2003). Hence modification by cross linking increases the
with adipic acid, ammonium phosphate, sodium acetate gel temperature of modified starches. This trend is shown
neutralized with fumaric acid and sodium acetate in Table 1 as all modified starches had higher gel
respectively. It is necessary that the pH of starch tends temperatures than the native starch. The addition of adipic
towards neutrality so that it can be used in industries acid and fumaric acid respectively to the sodium acetate
where a change in the pH of products is not desired. This, modified starch reduced the reaction efficiency of the
modification by cross-linking achieved with improved pH modification as observed in the reduction of their gel
values of the native starch to desirable limits of neutrality. temperatures. Similar thermal properties for cross-linked
wheat starch were also reported by Choi and Kerr (2004).
4.3 Moisture Content They indicated that the extent of the changes depends on
the botanic source of the starch, concentration; type of
The moisture content of starch is the amount of moisture cross-linking reagent and the reaction condition (Chel-
present in it. The higher the moisture content the lower Guerrero and Betancur, 1998).
the amount of dry solids in the flour. The maximum
allowable limit for moisture in starch flour is 14% 4.5 Swelling Power, Swelling Volume and
(Austin, 1984). Higher values promote growth of Solubility Of Samples
organisms which causes odours and off-flavour. Table 1
show that modification by cross-linking increased the When an aqueous suspension of starch is heated, as the
moisture content of the modified starches except for temperature increases and exceeds gelatinization

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 International Journal of Engineering and Technology (IJET) – Volume 2 No. 6, June, 2012

temperature, the starch granules become weakened and (2003) also indicated that the cross-linkages may reduce
the intermolecular bonds of the starch molecule become the movement of starch molecules, causing reduction in
distorted. This enables water molecules to become more water solubility and water absorption of cross-linked
attached to the starch molecules. The granules continue to starch.
swell as they absorb more water (Gunarantne and Corke,
2007). Cross-linking has been reported to decrease 4.6 Viscosity
(depending on the type of cross-linking agent and degree
of cross-linking) the swelling power, swelling volume and The viscosity of a substance is defined as its resistance to
solubility of starches from various sources (Hoover and flow and increases as temperature decreases or decreases
Sosulski, 1986). All modified starches show a decrease in as temperature increases (Coulson and Richardson, 2004).
their swelling power and swelling volume compared to Starch paste viscosity can be increased or reduced by
the native starch as shown in Table 1. The solubility of applying a suitable chemical modification (Agboola et al.,
starch is the water binding capacity of the starch. Table 1 1991). Increasing the level of cross-linking has been
shows that the native starch sample has zero percent reported to reduce or may completely prevent granule
solubility. This is because the granules have not been swelling which results in a decrease in viscosity
tampered with or ruptured. Results from modification by (Strivastava and Patal, 1973). The viscosity-temperature
cross-linking in Table 1 show an increase in solubility of behaviour of the native and modified starch samples are
all modified starches with sodium acetate modified starch shown in Figure 2. The results show that modification by
having the highest solubility of 66.67% showing an cross-linking improved (reduction in viscosity) the
increased randomness in the structure of the starch and the viscosity of the native starch. All the modified starches
rupture of the starch granules. The starch modified with show a decrease in viscosity at all temperatures compared
sodium acetate neutralized with fumaric acid has the to the un-modified native starch. The viscosity of native
lowest solubility among the modified starches. Singh et., starch, ammonium phosphate and sodium acetate
al (2007) also reported a reduction in solubility and modified starches increase as temperature decreases while
swelling of various cross-linked starch systems. They the modified starches with sodium acetate neutralized
have indicated that the resistance of a cross-linked starch with adipic and fumaric acids respectively gave unstable
towards solubility and swelling increases by increasing viscosity-temperature behaviour.
the concentration of cross-linking agent. Wang and Wang

Figure 2: Variation of Native and Modified Starch Samples with Temperature.

5. CONCLUSION Modification by cross-linking using four different

reagents (ammonium phosphate, sodium acetate, sodium
Improvements in the functional properties of a Nigerian acetate neutralized with adipic acid and sodium acetate
variety of native cassava starch were performed. neutralized with fumaric acid) was used to produce four
grades of modified starches. The modified starches
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 International Journal of Engineering and Technology (IJET) – Volume 2 No. 6, June, 2012

showed improvements in functional properties such as ash [2] Alejandro, A., Felipe, G., Francisco, J., Juscelino, T.
content, pH, moisture content, gelatinization temperature, and Luis, A. B. (2008), Physicochemical and
swelling power (influences texture) and volume, solubility Functional Properties of Cross-linked Banana
(enhances digestibility) and viscosity. Resistant Starch. Effect of Pressure Cooking, Starch,
Starch modified with sodium acetate had the best 60, (6), 286-291
improvement of the functional properties of the native
starch. This starch had low ash content, fairly neutral pH, [3] Association of Official and Analytical Chemists
the highest gel temperature, lowest moisture content and (AOAC), (1984), 14th Edition Washington DC.
highest solubility. The increased gel temperature gives
stronger inter-molecular bonds and makes this starch [4] Austin, G. T. (1984), Shreve’s Chemical Process
more resistant to shear stress and retrogradation. All other Industries, Fifth Edition, McGraw-Hill Book
modified starches showed varying degrees of Company, pp 567.
improvements in most functional properties investigated.
[5] Chel-Guerrero, L. and Betancur, A. D. (1998), Cross-
The starch modified with ammonium phosphate also linkage of canavalia ensiformus starch with adipic
showed an increase in gel temperature, increase in acid: chemical; and functional properties, Journal of
solubility and a decreased starch viscosity with a neutral Agricultural and Food Chemistry, 46 (6) 2087-2091.
pH. However, the starch modified with sodium acetate
mixed with adipic acid also showed an increase in gel [6] Choi, S. G. and Kerr, W. L. (2004), Swelling
temperature and an increased solubility, the viscosity of characteristics of native and chemically modified
this starch sample is quite unstable and has undesirable wheat starches as a function of heating temperature
characteristic for starch to be used in industries. This and time, Starch, 56, 181-189.
starch has a pH of 5.66. Starch modified with sodium
acetate and fumaric acid has an unstable viscosity, [7] Cock, J. H. (1982), Cassava: A basic energy source in
increased gelatinization temperature and solubility. This the tropics, Science, Vol, 218, no 4574, 755-762.
starch also has a neutral pH of 7.13.
[8] Coulson, J. M. And Richardson, J. F. (2004),
These starches can be used in industries where such starch Chemical Engineering, Vol. 1, 6th Edition,
properties are desired. It is recommended that starch Butterworth-Heinemann, Woburn, M.A
modified with sodium acetate and ammonium phosphate
can be used in the paper, paint and adhesives industries [9] Daramola, B. and Osanyinlusi, S. A. (2006),
because of its resistance to shear stress and low viscosity Investigation on modification of cassava starch using
suitable for surface sizing, coatings and for high quality active components of ginger roots (Zingiber
papers. The increased gelatinization temperature and low officinale Roscoe), African journal of Biotechnology,
viscosity of the modified starches made it also suitable for 5 (10), 917-920
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ACKNOWLEDGMENTS [11] Gunarantne, A. and Corke, H. (2007), Functional

properties of hydroxypropylated cross linked tuber
We acknowledge the following for their contributions and root starches, Cereal Chem, 84, 30-37.
towards the success of this research. The Faculty of
Agriculture, Rivers State University of science and [12] Hirsch, J. B. and Kokini, J. L. (2002), Understanding
Technology for providing the cassava specie used in this the mechanism of cross-linking agents (POCl3,
study, the Departments of Chemical/Petrochemical STMP, and EPI) through swelling behavior and
Engineering and Food Science for the use of their pasting properties of cross-linked waxy maize
laboratory for the conduct of the various experiments and starches, Cereal Chem, 79, 102-107.
analysis.
[13] Hoover, R. (2001), Composition, molecular structure,
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