ACTA

ACTA
UNIVERSITATIS
UNIVERSITATIS
CIBINIENSIS
CIBINIENSIS

10.2478/aucft-2018-0009 Series
SeriesE:
E:Food
Foodtechnology
technology

PROCESS OPTIMIZATION FOR DIETARY FIBER PRODUCTION FROM

CASSAVA PULP USING ACID TREATMENT

– Research paper –

Yanuar Sigit PRAMANA1, Titi Candra SUNARTI, PURWOKO

Agroindustrial Technology Department, Faculty of Agricultural Technology, Bogor

Agricultural University, Dramaga, Bogor, West Java, 16680, Indonesia

Abstract: Cassava pulp, the side product of tapioca industry consists of starch and fiber as the major component.
Acid treatment was employed in the conversion process of cassava pulp into dietary fiber to remove the starch
component, to increase fiber content, and to modify the structure of fiber. This study purposed to obtain optimum
process conditions (acid concentration, temperature, and reaction time) in the production of dietary fiber from
cassava pulp. Process optimization was conducted using Response Surface Methodology (RSM) for maximizing
Total Dietary Fiber (TDF), Water Holding Capacity (WHC) and Oil Holding Capacity (OHC) as the responses.
The optimum process was gained at 6% H2SO4 concentration, 127oC, and 45 mins. Prediction values of TDF,
WHC, and OHC were 100%, 10.47 g/g, and 3.60 g/g, respectively. Validation was carried out and resulted in TDF
96.95%, WHC 10.47 g/g, and OHC 3.55 g/g. Physicochemical properties of the resulting dietary fiber were
significantly improved. The fiber structure has modified which characterized by the changes in morphology and
crystallinity.

Keywords: cassava pulp, dietary fiber, optimization, acid treatment, physicochemical properties

INTRODUCTION polysaccharide that can not be digested in the

intestine but it can be metabolized by bacteria
Cassava pulp is a typical solid residue of tapioca that are located and through the digestive tract
production which is abundant in Indonesia but it (AACC, 2001). Dietary fiber has good health
has not been processed and utilized optimally. In implications for preventing chronic illnesses
2013, the amount of cassava processed to tapioca such as colon cancer, diabetes mellitus, and heart
was about 7.8 million tons in Indonesia (CDMI, illness (Lv et al., 2017). The competitiveness of
2014). It generated 780,000-1,170,000 tons dry fiber-fortified food product markets makes the
cassava pulp and increased every year. Due to its exploration of alternative sources of dietary
large amount, cassava pulp will become a fiber, especially from byproducts of food
pollution if it is not handled or processed further. processing industries become important (Elleuch
Recently, the utilization of cassava pulp in et al., 2010). Recently, Lv et al. (2017) have
Indonesia is still limited as fermentation studied dietary fiber from the core of maize
substrate, animal feed component, mosquito coil straw.
raw material as well as sauce raw material and Cassava pulp should be treated in a certain way
included as byproducts with low economic in order to have functional properties as dietary
value. fiber. Preparation of dietary fiber from cassava
Cassava pulp contains 55.5% starch and 35.2% pulp can be carried out with enzymatic or acid
total dietary fiber (Chaikaew et al., 2012). With treatment. The treatment is performed to reduce
its ample fiber content, cassava pulp is very starch component from about 60% to 15%
potential to be used as a fount of dietary fiber. In (maximum), and to increase TDF from about
addition, another advantage is that cassava pulp 30% to 70% (minimum) (Lacourse et al., 1994).
has very low-fat content; it is around 0.12% The weakness of the enzymatic method is that
(Sriroth et al., 2000) to 1% (Chaikaew et al., the slurry concentration of cassava pulp is very
2012), so it can avoid the problem of rancidity low, only 5-10% w/v (Lacourse et al., 1994) so
during storage. Dietary fiber is the the process is inefficient. At high substrate
1
Corresponding author. E-Mail address: [email protected]

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Vol. XXII (2018), no. 2
concentrations, the slurry of cassava pulp was conducted in order to maximize TDF, WHC,
becomes very thick at its gelatinizing and OHC. In addition, chemical composition,
temperature and this is not proper to the morphological structure, crystallinity and
use/action of the α-amylase enzyme (Srikanta et physicochemical properties of cassava pulp and
al., 1987). The use of cassava pulp substrate at obtained dietary fiber were also analyzed.
high concentration (20-50%) in the hydrolysis Process optimization was carried out using
process can be performed using an acid catalyst Response Surface Methodology (RSM). RSM is
(Ahmed et al., 1983; Srikanta et al., 1987). The an efficacious statistical method to obtain
acid treatment is expected to modify the fiber optimal process variables that improve the
structure to improve its functional properties. In responses (Fan et al., 2008). The experiment was
addition, acid catalyst requires a relatively arranged using the central composite design
cheaper cost. (CCD). The advantage of CCD is that the
In this study, the effects of acid (H2SO4) number of runs of experiments is fewer but
concentration, temperature and time of reaction accurate data can be generated for optimization
on the Total Dietary Fiber (TDF), Water Holding so the cost and time are more efficient than other
Capacity (WHC), and Oil Holding Capacity designs (Anderson and Whitcomb, 2005).
(OHC) were investigated. Process optimization

MATERIALS AND METHODS using CCD with 3 factors as independent

variables: sulfuric acid concentration,
Material: Cassava pulp was obtained from CV temperature and time of reaction. The fixed
Semangat Jaya, medium-scale tapioca industry variable chosen was cassava pulp slurry
in Lampung Province, Indonesia. Sulfuric acid concentration (30%w/v). The levels of the
(H2SO4), NaOH and other chemicals for analysis independent variable are reaction temperature
were purchased from Merck. (lower level 107oC; upper level 127oC), reaction
time (lower level 15 minutes; upper level 45
Raw material preparation: Cassava pulp minutes), and concentration of H2SO4 to the
output from tapioca industry extractor (± 85% weight of cassava pulp substrate (lower level
moisture content) was squeezed using screw 2%v/w; upper level 6%v/w). The function of this
press until ± 50% moisture content and dried optimization process was to maximize TDF,
with sun drying in order to have ≤13% moisture WHC, and OHC.
content. The dried cassava pulp was milled and
sieved with 40 mesh size. Statistical analysis of the data: Experimental
design arrangement and data processing were
Dietary fiber preparation: Preparation of done using Design-Expert® software 7.0.0. The
acidified water was performed by adding H2SO4 response surface and contour plot were used to
(ρ: 1.835 g/mL) at a certain volume (according show the effect of the factors on the responses
to the experimental concentration) into the water obtained. The coefficients on the empirical
(666 mL) in 2 L tank. Furthermore, the slurry model were estimated using multi-regression
was prepared by adding dry cassava pulp analysis. The significance of the empirical model
(particle size 40 mesh) of 200 g into the acidified obtained was tested using Analysis of Variance.
water. The reaction was carried out in the Optimization was performed using numerical
autoclave at the temperature and reaction time optimization.
according to the experimental design. After the
reaction completed, the slurry was filtered using Validation: It was carried out using the value of
a filter cloth and separated from the hydrolyzate independent variables obtained from the results
(sugar syrup). pH of cake (fiber) obtained was of numerical optimization. Furthermore, the
increased to pH 6 by adding NaOH 5%w/w, then actual response value was compared to the
washed and re-filtered. The fiber obtained was prediction response value.
dried at temperature 60oC until moisture content
being relatively constant. The dried dietary fiber Chemical composition analysis: Soluble
was milled and sieved at 100 mesh size. Dietary Fiber (SDF) and Insoluble Dietary Fiber
(IDF) were determined by the enzyme-
Optimization of dietary fiber production gravimetric method described by AOAC Official
process: The experimental design was arranged Methods 993.19 and 991.42. TDF was calculated

Pramana et al., Process optimization for dietary fiber production from cassava pulp 22
using acid treatment
by adding SDF and IDF. Moisture, protein, fat, 200 mg of sample was placed into a centrifuge
and ash content were determined using the tube, then 20 ml of distilled water was added.
method previously explained by AOAC (1995). The tube was incubated for 24 h in the water bath
Starch content was measured by the enzymatic shaker, then centrifugation at 3,000 x g for 60
method, through determination of glucose min was performed. The supernatant was
obtained from the saccharification using enzyme removed and the water content of the pre-
of α-amylase and amyloglucosidase (AMG). weighed pellet was measured by drying using an
Glucose was measured using the Spectroquant® oven at 120°C for 2 h. WHC of the sample was
UV-Vis pharo300 spectrophotometer using the stated as the weight of water held by one gram
dinitrosalicylic acid (DNS) method. of sample.
Oil Holding Capacity (OHC) measurement was
Morphology: The morphology of cassava pulp conducted using the method previously
and dietary fiber obtained were analyzed by described by Caprez et al. (1986).
scanning electron microscopy (EVO MA 10, Approximately 2 g of sample was placed in a 50
Carl Zeiss, Germany) at 1500x magnification. ml centrifuge tube, then 20 ml of corn oil was
The sample surface was coated with a thin gold added. The tube is left for 30 minutes at room
layer at 60 second sputter time and 20 mA temperature with agitation. Then, centrifugation
sputter current. Samples were fed into the SEM (2,500 x g, at room temperature for 30 mins) was
tool and the surface image was taken using the performed and the oil supernatant was poured
Secondary Electron (SE) detector, working and weighed. The OHC of the sample was stated
distance (WD) 8-9 mm and EHT 12.0 kV. as the gram of oil retained by one gram of
sample.
Crystallinity: The X-Ray Diffractogram and Cation-Exchange Capacity (CEC) was analyzed
crystallinity of the material were analyzed using according to Moorman et al. (1983).
X-Ray Diffraction. Measurements were Emulsifying Activity (EA) was determined
performed at 2Ɵ: 5-45° intervals, at 40 kV, 30 according to Yasutmasu et al. (1972). Viscosity
mA, and speed of 2° per min. was determined using viscometer. Swelling
Capacity (SC) was performed according to
Physicochemical properties analysis: Water Gómez-Ordóñez et al. (2010). Solubility
Holding Capacity (WHC) was measured using measurement was performed using the method
the procedure previously described by Suzuki et previously described by Paton and Spratt,
al. (1996) with minor modification. A total of (1984).

RESULTS AND DISCUSSIONS conversion to remove/decrease the starch

component and increase the TDF. Acid
Chemical composition of cassava pulp treatment could be employed to hydrolyze starch
In this study, the chemical composition (dry into sugar and to modify the structure of the fiber
basis) of cassava pulp consisted of 69.76% of from the crystalline structure to amorphous
starch, 27.40% of TDF (25.25% of IDF and structure.
2.15% of SDF), 1.37% of ash, 2.03% of protein
and 0.07% of fat. Similar observations were Optimization process by RSM
carried out by (Sriroth et al., 2000; RSM is a statistical technique that used to obtain
Rattanachomsri et al., 2009; Chaikaew et al., the best empirical model and problem analysis
2012; Virunanon et al., 2013; Zhang et al., on responses that are influenced by several
2016), which reported that cassava pulp variables and aims to obtain optimum responses
consisted of major components of starch and (Montgomery, 2008). From each of the
fiber. There was a small amount of protein, ash, predetermined levels of the factors, an
and fat. Cassava pulp generated in high experimental design constructed with CCD was
quantities as a side-product of tapioca industry is arranged using Design-Expert® 7.0.0 software
a potential source of biomass (Vaithanomsat et and shown in Table 1. TDF was selected as a
al., 2016). chemical quantitative response, whereas WHC
The starch component of cassava pulp has a and OHC are selected as the responses that
larger portion than the fiber component, while represent the quality (physicochemical
dietary fibers are components of non-starch properties) of dietary fiber products.
carbohydrates. It needs an appropriate

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Vol. XXII (2018), no. 2
Table 1. Experimental design and the values of observed responses
Factor 1 Factor 2 Factor 3 Response 1 Response 2 Response 3
Std A: C:
B:
order Concentration Time of TDF WHC OHC
Temperature
of H2SO4 Reaction % (g/g) (g/g)
(oC)
(%v/b) (mins)
1 2.00 107.00 15.00 72.07 6.74 2.11
2 6.00 107.00 15.00 73.15 7.33 2.12
3 2.00 127.00 15.00 85.09 10.43 2.89
4 6.00 127.00 15.00 94.20 10,.0 3.58
5 2.00 107.00 45.00 72.45 8.08 2.25
6 6.00 107.00 45.00 73.70 8.06 2.45
7 2.00 127.00 45.00 96.68 10.30 3.22
8 6.00 127.00 45.00 97.19 10.35 3.69
9 0.64 117.00 30.00 57.99 6.11 1.83
10 7.36 117.00 30.00 85.15 8.46 2.99
11 4.00 100.18 30.00 73.01 7.32 2.56
12 4.00 133.82 30.00 94.25 11.18 3.11
13 4.00 117.00 4.77 74.08 7.75 2.37
14 4.00 117.00 55.23 97.73 8.38 3.53
15 4.00 117.00 30.00 76.42 8.56 2.69
16 4.00 117.00 30.00 74.64 7.85 2.63
17 4.00 117.00 30.00 78.28 8.93 2.64
18 4.00 117.00 30.00 76.21 7.97 2.94
19 4.00 117.00 30.00 76.38 9.26 2.94
20 4.00 117.00 30.00 75.94 8.67 2.61

ANOVA of TDF response model indicates that of H2SO4 (A), temperature (B) and reaction time
TDF is a function of H2SO4 concentration (A), (C). The obtained model is a regression equation
temperature (B) and reaction time (C). By for a linear model as follow:
applying multiple regression analysis, it was Water Holding Capacity = 8.61 + 0.34A +
obtained the regression equation for the 1.31B + 0.21C (2)
quadratic model as follows: The linear model p-value of 0.0001 indicates a
Total Dietary Fiber = 76.23 + 4.22A + 8.60B significant model. There is only a possible
+ 4.05C + 0.91AB – 1.05AC + 1.71BC – 0.01% error in drawing conclusions. In this case,
2
1.16A + 3.10B2 + 3.91C2 (1) B is a significant component, which means that
The quadratic model p-value of 0.0033 indicates the temperature is a variable that significantly
a significant model. There is only a possible affects the WHC response. From the "Lack of Fit
0.33% error in drawing conclusions. p-value less test" of the model, it was obtained p-value
than 0.0500 indicates components of model are 0.1589> 0.05 indicates that the “Lack of Fit” is
significant. In this case, A, B, C, and C2 are not significant relative to the pure error. Non-
significant model components to the TDF significant “lack of fit” implies that the model is
response. The values of R2 (0.857) and R2adj good. The values of R2 (0.7227) and R2adj
(0.7283) indicate that the ability of the (0.6707) indicate that the ability of the
independent variable to explain the variance of independent variable to explain the variance of
the dependent variable is good (85.7% and the dependent variable is good enough (72.3%
72.8% respectively). “Adequate precision” is a and 67.1% respectively). An “adequate
measure to compare predicted design point precision” value of 12.571 (greater than 4)
values to the predicted mean error values. The indicates a model with high precision is eligible
value of “adequate precision” must be greater for use.
than 4.0, meaning that the model has high The ANOVA of OHC response model shows
precision (Kumari et al., 2008). “Adequate that the OHC is a function of the concentration
precision” value of 8.725 indicates an adequate of H2SO4 (A), temperature (B) and reaction time
signal that this model has a high precision and it (C). The obtained model is a regression equation
is eligible for use. for a linear model as follow:
The ANOVA of WHC response model shows Oil Holding Capacity = 2.76 + 0.24A + 0.39B +
that the WHC is a function of the concentration 0.21C (3)

Pramana et al., Process optimization for dietary fiber production from cassava pulp 24
using acid treatment
The linear model p-value of 0.0001 indicates a R2adj (0.667) indicate that the ability of the
significant model. There is only a possible independent variable to explain the variance of
0.01% error in drawing conclusions. In this case, the dependent variable is good enough (72.03%
A, B, and C are the significant model and 66.7% respectively). An “adequate
components to the OHC response. From the precision” value of 12.938 (greater than 4)
"Lack of Fit test" of the model, it was obtained indicates that this model has a high precision and
p-value 0.0505> 0.05 indicates that the “Lack of eligible for use. Response surface of the TDF,
Fit” is not significant relative to the pure error. WHC, and OHC and the effect of interaction
Non-significant “lack of fit” implies that the between variables can be seen in Figures 1(a)-(i).
model is good. The values of R2 (0.7203) and

Figure 1(a). Response surface of TDF on the effect Figure 1(b). Response surface of TDF on the effect of
of H2SO4 concentration and temperature H2SO4 concentration and time of reaction

Figure 1(c). Response surface of TDF on the Figure 1(d). Response surface of WHC on the effect
effect of temperature and time of reaction of H2SO4 concentration and temperature

Figure 1(e). Response surface of WHC on the effect Figure 1(f). Response surface of WHC on the effect
of H2SO4 concentration and time of reaction of temperature and time of reaction

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Vol. XXII (2018), no. 2
 Figure 1(g). Response surface of OHC on the Figure 1(h). Response surface of OHC on the effect of
effect of H2SO4 concentration and temperature H2SO4 concentration and time of reaction

Figure 1(i). Response surface of OHC on the effect of temperature and time of reaction

Optimization was performed by setting the Effects of acid concentration, temperature

condition of independent variables within the and reaction time on TDF, WHC, and OHC
experimental range and setting the TDF, WHC, Figure 1(a),(b),(c) show the interaction effects of
and OHC at maximum conditions. Several two factors on the TDF. The concentration of
optimization solutions were generated. From the H2SO4, temperature and reaction time had a
solution provided by the program, the optimal significant effect on TDF response, where each
solution has the maximum desirability value, in variable gave positive effect to increase TDF in
this case, 0.937 was selected as the best solution. experimental range. TDF is a fiber component
The optimum process conditions were obtained consisting of IDF (for instance cellulose,
at 6% H2SO4 concentration, 127oC temperature hemicellulose, and lignin) and SDF (pectin). The
and reaction time 45 mins, with prediction higher the temperature, the greater the TDF
response value of TDF 100%, WHC 10.47 g/g content of the product. This occurred because the
and OHC 3.6 g/g according to Figure 1. rate of starch hydrolysis reaction in the cassava
pulp also increased so that at the same time
Validation starch would be more hydrolyzed into sugar
Validation was performed at optimum process (Wahyudi et al., 2011). The hydrolysis reaction
condition. The actual responses value were TDF is an endothermic reaction that requires heat to
96.95%, WHC 10.47 g/g and OHC 3.55 g/g. The react, corresponding to the Arrhenius equation:
differences that occur between the predicted −𝐸𝐴
𝑘 = 𝐴𝑒 𝑅𝑇 (4)
values and the actual values at optimum
k = rate constant ; A = pre-exponential factor;
conditions were 3.1% for TDF, 0% for WHC and
EA= activation energy (J.mol-1); R = the gas
1.4% for OHC. The optimization result was
constant (J.mol-1.K-1); T = temperature (K).
acceptable because the actual values of TDF,
In addition, the longer reaction time the higher
WHC, and OHC were in accordance with the
TDF content of the product. Starch more
model prediction. This was indicated by three
hydrolysable into sugar during reaction time so
responses value meet the 95% confidence
the starch content in dietary fiber products
intervals presented by the program.
became less. The similar trend also occurred in
the variable of H2SO4 concentration. The higher

Pramana et al., Process optimization for dietary fiber production from cassava pulp 26
using acid treatment
the concentration of H2SO4, the activation maltose and maltose and can then break down
energy became smaller, and the reaction rate into glucose (Gaman and Sherrington, 1981).
constant became larger (Artanti and Andik, The process of acid hydrolysis will produce
2006). While the reaction rate increased, the hydrolyzate (by-products) which can be
starch hydrolyzed into sugars became more. separated from the fiber component in the
Then, TDF content increased when hydrolyzate cassava pulp. The hydrolyzate products need to
(sugar syrup) separated from the fiber. be detoxified to eliminate toxic compounds such
Figure 1(d),(e),(f) describe the interaction effects as furfural and HMF before used in applications
of the factors on the WHC. In this case, the in the industry. At high temperatures and
temperature was a variable that significantly pressures, the sugar from hydrolysis of starch
affected the WHC, whereas the H2SO4 and hemicellulose such as glucose, galactose,
concentration and reaction time had no and mannose is degraded into HMF and xylose
significant effect on the WHC. The higher the into furfural. HMF compounds can also be
temperature the WHC value increased. WHC derived from browning (Maillard) reactions
optimum achieved at temperature 127oC. between amino groups derived from proteins in
Figure 1(g),(h),(i) describe the interaction effects cassava pulp and glucose formed (Palmqvist and
of the factors on the OHC. The concentration of Hagerdal, 2000). Detoxification method using
H2SO4, temperature and time were the variables activated carbon is a good method with relatively
that significantly affected the OHC. There was a lower costs (Mussatto and Roberto, 2001). The
linear relationship between concentration of use of 5% activated carbon concentration could
H2SO4, temperature and reaction time with reduce HMF concentrations by 85% (Hodge et
OHC, where the increase of each variable would al., 2009).
increase the OHC value. In the previous
discussion, it was known that the increased Physicochemical functional properties
concentration of H2SO4, temperature and Physiological effects are correlated with the
reaction time would increase the TDF. The physicochemical properties of dietary fiber and
higher TDF content indicates that the fiber its fractions (Marsono, 2004). Dietary fiber
component which can absorb/retain oil will also specific properties associated with their
increase. The more oil retained the higher the physiological effects include fermentability,
OHC value. water-binding capacity, organic molecular
absorption, viscosity and ion exchange
Chemical composition of dietary fiber properties. Some physicochemical properties for
products this investigation are summarised in Table 2.
The chemical composition of dietary fiber Table 2 shows that there are significant
obtained from the optimization result was improvements of cassava pulp physicochemical
analyzed. Dietary fiber consisted of 2.7% starch, properties after conversion to dietary fiber
96.95% of TDF (94.36% of IDF and 2.59% of through acid treatment. The dietary fiber
SDF), and 1.3% of ash. The TDF content in obtained from optimization results has the
dietary fiber product increased significantly highest WHC, followed by barley bran, wheat
from originally 27.4% in cassava pulp (raw bran, and cassava pulp. Fiber especially IDF has
material), while the starch content in dietary the ability to hold the water (Marsono, 2004).
fiber decreased significantly from originally WHC and swelling capacity values follow the
69.76% in cassava pulp. This occurred because trend of fiber content in the ingredients. It was
the starch component of cassava pulp was found that dietary fiber had the highest TDF
hydrolyzed by acid as a catalyst into hydrolyzate content (96.95%), followed by barley bran and
in the form of sugar syrup which was then wheat bran, 54.83% and 31.73% (Matin et al.,
separated as a byproduct. 2013), respectively. WHC is a measure of the
Starch granules on the cassava pulp were trapped quantity of water held on to the fibers after
within the matrix by the fiber structure. To undergoing pressures as centrifugation (Nelson,
remove the starch granules, the acid through the 2001). WHC properties need to be measured
hydrolysis process will cut the polysaccharide before the dietary fiber is used as a functional
bonds, especially the starch with the α-1,4 food. OHC is a physicochemical property of
glycosidic bonds into smaller molecules fiber material that can be applied in food
sequentially. The starch molecule initially formulations. The porosity of fiber structures is
breaks into shorter chains of glucose called a a major factor affecting the ability of fibers to
dextrin. Dextrin has broken down again into retain oils (Nelson, 2001). In addition,

Acta Universitatis Cibiniensis Series E: FOOD TECHNOLOGY 27

Vol. XXII (2018), no. 2
hydrophobicity, the number of lipophilic sites due to the lower solubility and SDF content
and capillary appeal are also complex factors (2.59%). Gum and pectin are included in the
affecting OHC (Kinsella, 1976). Materials that SDF group. Many studies have shown that gum
have high OHC and emulsifying activity are able and pectin increase the viscosity of intestinal
to act as emulsifiers in formulated foods. The contents, whereas the IDF does not have that
dietary fiber obtained from optimization results property, but this fiber accelerates intestinal
showed the highest OHC and emulsifying emptying and transits throughout the intestine
activity values compared to barley bran and (Marsono, 2004). IDF raises the number of feces
wheat bran. The other important property of because it is resistant to bacterial degradation
dietary fiber is ability as an ion exchanger. This while the SDF is easily fermented by bacteria
property can be a negative characteristic of resulting in an increase of bacterial mass. The
dietary fiber because it can reduce mineral obtained dietary fibers have very high TDF
availability and absorption of electrolytes content with good physicochemical properties so
(Marsono, 2004). According to Carvalho et al. the product is suitable for use in food
(2009), sulfate content, uronic acid, and load applications for low-calorie diets, processed
density affect cation exchange capacity. The meats, fat replacer, emulsifying agents and for
dietary fiber obtained has a lower cation the bakery industry. Dietary fiber is appropriate
exchange capacity compared to barley bran and for reducing fat content in meat-based products
wheat bran. On the other hand, viscosity of the in order to obtain healthier food. In addition, the
fiber suspension related to the solubility, use of dietary fiber in meat products can improve
molecular weight, and structural chemical bonds the texture profile and characteristics associated
of the material (Choct, 2002). The dietary fiber with the cooking process (Tufeanu and Tita,
obtained from the optimization result showed 2016).
lower viscosity than barley bran and wheat bran,

Table 2. Physicochemical properties of cassava pulp, the dietary fiber obtained, wheat bran and barley
bran
Properties Cassava Pulp Dietary Fiber Wheat bran Barley bran
(Raw material) (Product (Matin et al. (Matin et al.
Obtained) 2013) 2013)
Water Holding Capacity (g/g) 2.97 10.47 3.41 4.57
Oil Holding Capacity (g/g) 1.36 3.55 1.21 1.79
Cation-Exchange Capacity (meq/kg) 3.7 12.7 16.9 29.9
Emulsifying Activity (%) 57 77.89 32.84 52
Viscosity (cP) 0.3 0.35 1.74 2
Swelling Capacity (ml/g) 6.35 11.47 5.75 8
Solubility (%) 0.45 0.53 - -

Morphology of 15 mins, possibly in the amorphous section.

The results of the morphological analysis of However, in this condition still visible that starch
cassava pulp and dietary fiber products are granules were bound to the fiber matrix. After
shown in Figure 2. The results showed that the acid treatment at 4% H2SO4 concentration;
starch granules in cassava pulp were bound in a 117oC; 30 minutes, the degradation process was
trapped position on the biomass fiber matrix more obvious, marked by the visible bundle of
(Figure 2a). Therefore, the grinding process can fibers that allegedly was the bundle of cellulose
be carried out to minimize particle size and fibers. Cellulose fiber was the most resistant
increase its surface area and to partially cut the cassava pulp component to the degradation
fiber matrix wrapping the starch granules. It may process, while the hemicellulosic component
increase access to hydrolyze starch granules was more soluble and degraded (Hermiati,
(Hermiati, 2012). Cassava pulp underwent 2012). At optimum process conditions (6%
gradual degradation during acid and heat H2SO4 concentration; temperature 127oC; and a
treatment as shown in SEM morphological 45 mins reaction time), the biomass matrix
image of cassava pulp after treatment (Fig. degradation was very clear. This was
2(b),(c),(d)). The biomass matrix was seen to be characterized by the formation of fiber bundles
slightly degraded at 2% H2SO4 acid treatment; with a regular structure. In this condition almost
reaction temperature 107oC; and a reaction time all starch was hydrolyzed and separated from the

Pramana et al., Process optimization for dietary fiber production from cassava pulp 28
using acid treatment
fiber matrix, so that resulted in dietary fiber with processing conditions are important things that
a porous fiber structure. Microstructure influence the physicochemical properties of
(porosity, particle size, and fiber length) and dietary fiber related to water (Nelson, 2001).

Figure 2. Scanning electron microscope image of : (a) untreated cassava pulp; (b) after treatment at 2% H 2SO4;
107oC; 15 mins; (c) after treatment at 4% H2SO4; 117oC; 30 mins; (d) after treatment at 6% H2SO4; 127oC; 45
mins

Crystallinity 23.3°. In other conditions, 4% H2SO4

X-ray diffractogram of cassava pulp before and concentration; 117oC; 30 mins, crystallinity in
after treatment is shown in Figure 3. X-ray the range 15° -18° decreased while the
diffractogram of cassava pulp before treatment crystallinity in the range 21°- 23° increased. At
shows that cassava pulp has a high peak at 2Ɵ by optimum process conditions (6% H2SO4; 127oC;
15°, 17°, 18° and 23°. This spectrum type is 45 minutes), crystallinity in the range 15° - 18°
similar to the tapioca starch spectrum that having more decreased while the crystallinity in the
a strong peak at 15°, 17°, 18° and 23° as reported range 21°- 23° more increased. It was possible
by Atichokudomchai et al. (2001). Starch and that the starch component was almost
fiber are the main constituents of cassava pulp, completely hydrolyzed, so the contribution of
each of which has crystallinity properties. The crystallinity came from the fiber component. The
result of X-ray diffraction analysis shows that spectrum under these conditions has the high
the crystallinity of cassava pulp used in this peak at 21°, 21.8° and 22.4° with the crystallinity
study was 45.13%. By treatment using 2% of 44.9%. By acid treatment, modification of the
H2SO4; reaction temperature 107oC; and reaction fiber structure was occurred and changed the
time of 15 mins, the crystallinity of the cassava crystalline structure into a more amorphous
pulp decreased to 36.19% due to the hydrolysis structure so as to increased its porosity and
of starch component. The spectrum under these improved the physicochemical properties.
conditions has the high peak at 21.4°, 22.4°, and

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Vol. XXII (2018), no. 2
 Figure 3. X-ray diffractogram of cassava pulp before and after treatment

CONCLUSIONS at H2SO4 concentration 6% (v/w), temperature

127oC and reaction time 45 mins. Temperature is
The results of this study indicate that cassava the variable that most influences the response of
pulp is a potential and valuable resource that can TDF, WHC and OHC. The results of this study
be converted to the dietary fiber using acid also proved that the acid treatment can be used
treatment. The acid treatment is effective for to modify the fiber structure and improve the
removing the starch component and increasing physicochemical properties. Therefore, cassava
the TDF content. The optimum process pulp can be an excellent choice for the
conditions for the production of dietary fiber are production of dietary fiber from biomass.

ACKNOWLEDGMENTS
This research work is supported by Agency for the Assessment and Application of Technology (BPPT),
as well as the Ministry of Research, Technology and Higher Education, Republic of Indonesia.

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