Optimization of Coconut (Cocos Nucifera) Milk Extraction Using Response Surface Methodology
Optimization of Coconut (Cocos Nucifera) Milk Extraction Using Response Surface Methodology
Email address:
anielijah@gmail.com (A. I. Elijah)
*
Corresponding author
Received: August 23, 2016; Accepted: September 3, 2016; Published: October 18, 2016
Abstract: Coconut milk provides health benefits due to its medium chain fatty acids and is widely utilized in the food
industry. However, there seems to be inadequate information on the optimal extraction conditions for coconut milk. In this
study, a response surface methodology (RSM) based on central composite design (CCD) was employed to optimize the
extraction time (X1), extraction temperature (X2) and particle size of coconut meat (X3) for coconut milk extraction. Yield, pH,
viscosity and total solid content of coconut milk were evaluated as responses. Regression models were generated and adequacy
tested with lack of fit test and coefficient of determination (R2). The results showed that extraction time; extraction temperature
and particle size of coconut meat had significant (p˂ 0.05) effects on responses. The R2 for yield, pH, viscosity, and total solid
content of coconut milk were 0.9976, 0.7352, 0.6748 and 0.9787 respectively. Optimum extraction time, temperature and
particle size of coconut meat with the highest desirability index of 0.797 was 15 min, 40°C and ≤ 1617 µm respectively, while
optimum yield, pH, viscosity, and total solid content of coconut milk were estimated at 61.129%, 6.6, 2.85 cp and 16.01%
respectively. The experimental results obtained validate the predicted model within the acceptable range of the responses. The
results also suggest that the obtained model is acceptable for the maximum milk yield and improved quality consistency.
Keywords: Coconut Milk, Optimization, Response Surface Methodology, Central Composite Design
fat has been reported to improve digestion and bowel responses (dependent variables).
function, support tissue repair and immune system functions, The two most common and popular designs in RSM are
help protect the body from breast colon and other cancers, central composite design (CCD) and Box- Behnken design
improve the cholesterol ratio, reduce the risk of heart disease BBD. Shishir et al. [21] reported that CCD is flexible and
and increase the metabolic rate of body fat, among other considered as most effective for uniform precision with lower
benefits [10]. The health benefits of coconut oil are mainly runs required, chronological investigation and reasonable
from the medium chain fatty acids (MCFAs). These MCFAs information for lack of fit test. Thus the aim of the present
are similar to that of human milk and have corresponding study was to determine the optimum parameters for
nutraceutical benefits. The most predominant MCFA is lauric extraction of coconut milk using RSM based on central
acid (45– 53%). This is converted in the body into a highly composite design.
beneficial compound called monolaurin, an antiviral and
antibacterial agent that destroys a wide variety of disease 2. Materials and Methods
causing organisms. Furthermore, the fats present in coconuts
are less likely to clog arteries, because the body does not 2.1. Materials
store coconut fats which makes coconut milk a healthy
alternative to cow’s milk when it comes to preserving heart’s Matured coconuts (7-8 months old) of the dwarf variety
health [11]. Consequently, the world market for coconut milk were collected directly from the trees in EmVic farm in
has increased from USD 1.2 billion in 2008 to USD 1.3 Ibesikpo Asutan Local Government Area, Akwa Ibom State,
billion in 2010 [12]. Nigeria.
In Nigeria, CM extraction is primarily done manually 2.2. Methods
which is very laborious. Besides, the extraction process has
not been standardized. To our knowledge, the optimal 2.2.1. Extraction of Coconut Milk
extraction conditions are not known. Different people extract The coconut was dehusked, cracked to separate the meat
under different conditions resulting in inconsistencies in from the shell while the coconut water was poured into a
product quality. The composition of CM, and by extension its container and stored for further use. The brown skin of the
quality, depends largely on the extraction procedure. It has coconut meat was removed and the meat thoroughly washed
been shown that the amount of water used for extraction, and grated using manual grater. The grater was fabricated
affects significantly the moisture and fat content of the milk by the Department of Food Engineering, University of Uyo,
[13]. Moreover, extraction time and temperature [14] have Nigeria, with particle size numbers ≤ 1311.93, ≤ 1617, ≤
been identified as important factors in CM extraction. 2353.5, ≤3090 and ≤ 3395.07 µm. The grated coconut meat
Agarwal and Bosco [15] showed that the extraction was mixed in a ratio of 1:1 with a solution containing 75%
efficiency of CM was enhanced by enzyme, thus, aiding in distilled water and 25% coconut water and allowed to stand
rupture of coconut meat cell walls and subsequent leaching in a water bath at stipulated temperatures and time
of the milk. It is believed that other factors such as extraction according to the CCD (Table 1). The slurry was then
time, extraction temperature and particle size of coconut pressed and filtered through cheese cloth to remove the
meat could have great influence on the quality of CM. solid residue and recover the milk. The milk was
One of the recent techniques being used for development pasteurized at 90°C for 30 min and allowed to assume room
of optimum food products to enhance their nutritive and temperature (37°C).
product quality is process optimization using response
surface methodology (RSM). RSM is a collection of Table 1. Experimental range and levels of the independent variables.
mathematical and statistical techniques useful for the Coded levels
Independent Variable
modeling and analysis of problems in which a response of Symbol – -1 0 +1 +
interest is influenced by several variables and the objective is
to optimize this response [16]. RSM considers interaction Time (min) X1 7.92 10 15 20 22.07
among process parameters and optimize them to a reasonable Temperature (°C) X2 35.85 40 50 60 64.14
range, with the advantage of the relevant information in the Particle size (µm) X3 1311.93 1617 2353.5 3090 3395.07
shortest time with the least number of experiments [17].
Many researchers have employed RSM to optimize processes 2.2.2. Physicochemical Analysis
in the food systems as a mathematical model with the Samples were evaluated for percentage yield, pH, viscosity
objective of achieving product excellence at the lowest and total solid content. Percentage yield was expressed as:
possible overall cost and accelerate the transitional cycle
from research and development to manufacturing [18]. RSM Y (%) = W2 / W1 x 100 (1)
has been widely reported for the optimization of a wide range Where W2 = weight of coconut milk extracted; W1 =
of products such as; extraction of olive oil [19], coconut oil weight of grated coconut meat + extraction solution added
[15], and has been found to be effective tool in optimizing About 100 ml of sample was poured into a beaker and
any process [20] wherein the interaction among factors thoroughly mixed. pH was measured using a pH meter
(independent variables) has to be tailored for desired (Model Voltcraft pH-100 ATC, USA). The viscosity of the
International Journal of Nutrition and Food Sciences 2016; 5(6): 384-394 386
coconut milk samples was determined using Fann Viscometer 2.3. Experimental Design and Statistical Analysis
(Model 35SA, USA). The sample was placed in the
viscometer cup. The cup was raised until the spindle was A Central Composite Design (CCD) of Response Surface
properly immersed. The Fann Viscometer was set at 600 rpm Methodology (RSM) was used to optimize the extraction
and readings were taken after 120 s of rotation and expressed variables and to study the interaction of process variables.
in centipoise (cp). There were 3 independent variables; extraction time (X1),
Total solid (TS) content of the coconut milk was extraction temperature (X2) and the particle size (X3) of
determined using the Association of Official Analytical coconut meat. Each variable had 5 different coded levels
Chemists [22] method. Two (2) ml of the sample was (Table 1) from low (-1), to medium (0) and high (+1) as well
measured into a previously weighed evaporating dish. The as star points (± ) for efficient determination of curvature
dish containing the sample was heated in an oven at 105°C. and quadratic term. Dependent variables such as yield, pH,
The sample was dried to a constant weight and then cooled in total solid and viscosity of coconut milk were evaluated as
a desiccator and reweighed. The weight of the solid was responses for the factors studied. The experimental design in
estimated by difference and expressed as the percentage of the actual levels of variables is shown in Table 2. All
the sample weight. TS content was calculated as follows: experiments were performed in triplicates. Statistical analysis
for coconut milk extraction was performed using Design
TS % = × 100 (2) Expert (Stat-Ease Inc., Minneapolis, MN, USA) software
version 9.0. The experimental data were fitted to a quadratic
Where W1 = Weight of empty dish, W2 = Weight of dish + model to express the response variables as a function of the
dried sample, W3 = weight of sample, TS = total solids. independent variables using equation (3).
Y = βo + β1X1 + β2X2 + β3X3 + β12 X1X2 + β13X1 X3 + β23 X2X3+ β11 X12 + β22 X22 + β33 X32 (3)
Where Y is the desired value of response; X1, X2, X3 are extraction temperature and particle size of coconut meat on
independent variables; βo is the constant; β1, β2, β3 are coconut milk yield, pH, viscosity and total solid content are
coefficients of linear regression; β12, β13, β23 are coefficients presented in Table 2. These experimental data were used in
of interaction regression and β11, β22 and β33 are coefficients RSM program to generate the best predicted model and its
of quadratic regression. The lack of fit of the model was statistical analysis. The quadratic model with the lowest
evaluated and the model adequacies were assessed using standard deviation, highest R2, adjusted and predicted R2
coefficient of determination (R2), adjusted R2, predicted R2, values were observed to be significant (p<0.05) and effective
adequate precision and coefficient of variation (CV). The in describing the effect of independent variables on yield and
analysis of variance (ANOVA) tables were generated and the total solid content of coconut milk. On the other hand, pH
effect and regression coefficients of individual linear, and viscosity were modelled with reduced two factor
quadratic and interaction terms were determined. The interaction (2FI) and linear model respectively. Sudamalla et
significance of all terms in the polynomial were judged al. [23] reported that in order to develop a regression model
statistically at 5% level of probability (p<0.05). that is statistically significant, the insignificant terms are
removed from the model thus resulting in a model’s
3. Results and Discussion (reduced) efficiency in describing response. The fitted
regression models, in terms of coded factors are shown using
3.1. Model Fitting polynomial equations as follows:
where Y1 = yield, X1 = extraction time, X2 = extraction temperature and X3 = particle size of coconut meat.
Table 2. Design matrix of central composite design obtained from RSM and experimental values of the responses for coconut milk extraction.
PY = Predicted yield, Y1 = Observed yield, Vis = Viscosity, TS = Total solid content, X1 = Extraction time, X2 = Extraction temperature and X3 = Particle size
of coconut meat, a mean ± standard deviation and n =3
Table 3. Analysis of variance (ANOVA) for the fitted polynomial model of the dependent variables.
The fitness of the final predicted polynomial model was the goodness-of-fit of the model was also ascertained by the
considered based on the results of analysis of variance coefficient of determination (R2) shown in Table 4. Jusoh et
(ANOVA). Result in Table 3 showed that the probability al. [25] reported that the best R2 value for a good model
value (p-value) of the response models was less than 0.01, fitting was estimated between 0.8 and 1.0. However, R2 <
suggesting that the models for the responses were statistically 0.80 had been reported by Gupta et al. [24], indicating a fair
correct and effective with insignificant lack of fit for pH and fit of the model, but reliable in making predictions.
viscosity. There was no F-value for lack of fit for yield which Consequently, R2 of 0.7352 and 0.6748 for pH and viscosity
showed that, lack of fit for the model had neither a significant respectively indicated fair fit of the models. This implied that
nor a non-significant effect on the response [24]. In addition, only 73.52% of variations in pH and 67.48% variations in
International Journal of Nutrition and Food Sciences 2016; 5(6): 384-394 388
viscosity were explained by 2FI and linear model reliable. This implies that the fitted models of responses were
respectively, while over, 97% variations in yield and total highly reliable and can be considered reasonably
solid were explained by quadratic model. reproducible. The predicted R2 was in reasonable agreement
Results in Table 4 revealed that coconut milk yield, pH and with the adjusted R2. This is because the difference between
TS had low coefficient of variation (CV) values (<3.5). CV is them was less than 0.2, which illustrated that there were
a measure of deviation from the mean values, which shows excellent correlations between the independent variables in
the reliability of the experiment. CV also describes the extent predicting the responses. Adequate precision is a comparative
to which the data were dispersed as well as the measure between the predicted values and the mean predicted
reproducibility and repeatability of the model [26]. Shishir et error and measures the signal to noise ratio. A ratio greater
al. [21] reported that a CV ˂ 10% indicates better precision than 4 is desirable. Our results (Table 4) showed that
and reliability while Gupta et al. [24] reported that CV > adequate precision values were greater than 4; therefore the
10% indicated that the experiment was less precise but respective models can be used to navigate the design space.
Table 4. Estimated regression coefficients of the fitted polynomial model representing the relationship between responses and process variables at the design
response surface.
3.2. Effect of Extraction Time, Extraction Temperature and meat, extraction time and extraction temperature, quadratic
Particle Size of Coconut Meat on the Yield of Coconut terms of extraction time, extraction temperature and particle
Milk size of coconut meat had significant (p<0.05) effects on the
yield of coconut milk. A positive and negative coefficient of
The result in Table 2 showed that the predicted and the independent variables in the model represents synergistic
observed coconut milk yield varied from 53.49 to 61.84% and antagonistic effects respectively.
and 53.33±0.33 to 61.67±0.30% respectively. The highest The main effect of time (Figure 1a) indicated that increase
yield (61.67±0.30%) of coconut milk was obtained during in extraction time resulted in increased milk yield. This result
extraction at 50°C, for 15 min using particle size 1311.93 µm is in agreement with the reports of Agarwal and Bosco [15]
(run 12), which also had the highest total solid content who reported increased coconut milk yield with increased
(17±0.38%). The yield of coconut milk was found to be a time; and that of Deswal et al. [27] who reported increased
function of the linear, interactions and quadratic effects of the milk yield during the extraction of oat milk using response
independent variables. Result showed that extraction time, surface methodology. Figure 1a also showed that increase in
extraction temperature, particle size of coconut meat, extraction temperature and extraction time resulted in increase
interactions of extraction time and particle size of coconut in yield of coconut milk. This is because the rise in
meat, extraction temperature and particle size of coconut temperature with time increases the diffusion of the milk solids
389 Victor Ephraim Edem and Aniekpeno Isaac Elijah: Optimization of Coconut (Cocos nucifera) Milk
Extraction Using Response Surface Methodology
while decreasing the viscosity [19]. The mass transfer 3.4. Effect of Extraction Time, Extraction Temperature and
coefficient of the extraction process also increases with Particle Size of Coconut Meat on the Viscosity of
temperature thus effecting the diffusion of the milk. The Coconut Milk
positive linear term for time and negative quadratic time
suggests that the effect of time resulted in increase in milk The viscosity of coconut milk ranged from 1.5±0.10 to
yield until a turning point (16 min) was reached beyond which 3.0±0.10 cp. ANOVA showed that viscosity was significantly
time had a negative impact on yield. The quadratic term (p<0.05) affected by particle size of coconut meat, whereas
exerted a downward force on the yield, indicating that there extraction time and extraction temperature had no significant
was less than linear increase in yield with regards to time (p>0.05) effect on the viscosity of coconut milk. The
thereby resulted in a slight tilting of the surface (Figure 1a). negative coefficient of particle size indicated that particle
The result also showed that the yield of coconut milk size of coconut meat exerted an antagonistic (negative) effect
increased with decrease in particle size of coconut meat and on viscosity. This implied that viscosity of coconut milk is a
increase in extraction time (Figure 1b). The increase in milk function of linear effect of particle size of coconut meat. The
yield could be attributed to the diffusion of water-soluble 3-D plot of RSM (Figure 3) shows that increase in particle
components of the coconut meat [15]. Smaller particle size of size of coconut meat led to sharp decrease in viscosity of
coconut is an indication that the coconut meat cell walls had coconut milk. Similarly, smaller particle size of coconut meat
been ruptured in a degree that led to a larger surface area resulted in more viscous milk than larger particles.
which in turn led to increase in the efficiency of the release 3.5. Effect of Extraction Time, Extraction Temperature and
of the components from the cells. More milk solids were Particle Size of Coconut Meat on Total Solid Content
extracted from smaller particle size due to the bigger of Coconut Milk
interfacial area of the solid. The shorter distance the solvent
has to travel to extract the milk from the solid increases the Table 2 showed that the total solid content ranged from
pore diffusion between solid and solvent. The larger particle 8.62±0.10 to 17.0±0.38%, indicating that the variation
has a smaller contact surface area and is more resistant to between the maximum and minimum value of total solid
solvent entrance and milk diffusion [28]. These findings are content was 8.38% during extraction at different process
in agreement with the report of Agarwal and Bosco [15] who variables. Particle size of coconut meat, interaction effect of
also observed increase in milk yield with decrease in particle extraction time and extraction temperature, as well as the
size during viscozyme - L. assisted extraction of coconut quadratic terms of time and particle size of coconut meat had
milk and virgin coconut oil. significant (p<0.05) effects on total solid content of coconut
Effect of particle size of coconut and temperature on the milk. The negative coefficient of effect of particle size of
yield of coconut milk is presented in Figure 1c. The positive coconut meat showed that particle size of coconut meat had a
coefficient of the interaction effect of extraction temperature negative effect on total solid content of coconut milk. Also,
and particle size of coconut meat resulted in increased the positive coefficient of interaction of extraction time and
coconut milk yield. This may be attributed to the fact that the extraction temperature indicated a synergistic effect on total
leaching of water soluble components from coconut meat solid content of coconut milk (Figure 4a). Figure 4a showed
was facilitated at higher temperatures thus resulting in that increase in temperature and time of extraction resulted in
increased milk yield. Therefore, increase in particle size with an increase in the total solid content of coconut milk.
temperature resulted in a slight increased milk yield. Increased time and temperature of extraction may aid the
dissolution of more soluble solid of coconut meat into the
3.3. Effect of Extraction Time, Extraction Temperature and surrounding solution thus resulting in increased total solid of
Particle Size of Coconut Meat on the pH of Coconut the milk. However, Murevanhama [30] reported a decrease in
Milk total solid of bambara groundnut milk with increased time
The pH of coconut milk ranged from 6.59±0.01 to and temperature. This disparity in total solids content may be
7.0±0.10 (Table 2). Extraction time and extraction as a result of differences in molecular organization of the
temperature had significant (p<0.05) effect on the pH of biological material as well as the extraction time (2-6 h)
coconut milk. The result showed that pH was found to be a employed by the different researchers. The negative
function of linear terms of extraction time and extraction quadratic time indicated that the effect of time resulted in
temperature, with a mean pH of 6.74. This result is in increased total solid until a turning point (16 min) was
agreement with that of Aidoo et al. [29] who stated that reached beyond which time had a negative effect on total
vegetable/plant milk was slightly acidic with a pH range of solid. This effect is seen by the tilting of the response surface
6.33 to 6.97 and more than half of the total extraction process plot in Figure 4a. Figure 4b revealed that particle size exerted
variables tested were within this range. The positive main a decline in total solid content of coconut milk. Increase in
effect of the extraction time and temperature indicated that the particle size of coconut meat resulted in decrease in total
increase in extraction temperature from 40 – 60°C and solid content with time. Increase in particle size of coconut,
extraction time from 10 – 20 min (Figure 2) aided in the led to a smaller surface area as some components of the
dissolution of the coconut components, which resulted in an coconut are locked up in the vegetative cells resulting in low
increased pH of coconut milk. total solid content. Similarly, increase in particle size also led
International Journal of Nutrition and Food Sciences 2016; 5(6): 384-394 390
62
60
58
56
Yield (%)
54
52
50
60 20
55 18
16
50
14
45
Temperature (DegC) 12 Time (min)
40 10
62
60
58
56
Yield (%)
54
52
50
20
18
3090 16
2795.4
14
2500.8 Time (min)
2206.2 12
1911.6
1617 10
Particle size (micron)
62
60
58
56
Yield (%)
54
52
50 60
55
3090 50
2795.4
2500.8 Temperature (DegC)
2206.2 45
1911.6
1617 40
Particle size (micron)
Figure 1c. Effect of particle size of coconut meat and temperature on the yield of coconut milk.
391 Victor Ephraim Edem and Aniekpeno Isaac Elijah: Optimization of Coconut (Cocos nucifera) Milk
Extraction Using Response Surface Methodology
7.1
6.9
6.8
6.7
pH
6.6
6.5
6.4
20 60
18 55
16
50
14
45
Time (min) 12 Temperature (DegC)
10 40
3.5
3
Viscosity (Cp)
2.5
1.5
20
18
16 3090
2795.4
14
Time (min) 2500.8
12 2206.2
1911.6
10 1617
Particle size (micron)
Figure 3. Effect of extraction time and particle size of coconut meat on the viscosity of coconut milk.
20
18
16
14
Total solid (%)
12
10
60 20
55 18
16
50
14
45
Temperature (DegC) 12 Time (min)
40 10
Figure 4a. Effect of time and temperature on the total solid content of coconut milk.
International Journal of Nutrition and Food Sciences 2016; 5(6): 384-394 392
20
18
16
14
Total solid (%)
12
10
8
20
6
18
16
20
18
16
14
Total solid (%)
12
10
8
60
6
55
50
3090 Temperature (DegC)
2795.4
2500.8 45
2206.2
1911.6
1617 40
Particle size (micron)
Figure 4c. Effect of particle size of coconut meat and extraction temperature on total solid content of coconut milk.
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Values
Response a
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