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International Journal of Biological Macromolecules 73 (2015) 202–206

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International Journal of Biological Macromolecules


journal homepage: www.elsevier.com/locate/ijbiomac

Process variables influence on microwave assisted extraction of


pectin from waste Carcia papaya L. peel
J. Prakash Maran a,∗ , K. Arun Prakash b
a
Department of Food Technology, Kongu Engineering College, Perundurai, Erode 638052, TN, India
b
Department of Mathematics, Kongu Engineering College, Perundurai, Erode 638052, TN, India

a r t i c l e i n f o a b s t r a c t

Article history: The objectives of the present study were to evaluate and optimize the influence of process variables
Received 10 September 2014 such as microwave power, pH, time and solid–liquid ratio on the extraction of pectin from waste Carcia
Received in revised form 5 November 2014 papaya L peel. The experiments were carried out based on a four factors three level Box-Behnken response
Accepted 10 November 2014
surface design. A quadratic model was developed from the experimental data in order to predict the pectin
Available online 18 November 2014
yield. The optimal condition was found to be: microwave power of 512 w, pH of 1.8, time of 140 s and
solid-liquid ratio of 1:15 g/ml with maximum pectin yield (25.41%).
Keywords:
© 2014 Elsevier B.V. All rights reserved.
Extraction
Pectin
Waste Carcia papaya L peel

1. Introduction spite of all these advantages, consumption of these fruits generates


a great amount of wastes and by-products (either at the farmer,
Carica papaya L. (papaya) is a large perennial tree-like but herba- at the processing industry, or from retail), including outer skin
ceous fruiting plant from the Caricaceae family. Papaya is a delicious wastes that can produce environmental pollution if not properly
tropical fruit which has a great taste, mouthwatering flavor and handled. Usually, the peels are considered as waste, although they
great health benefits. Originally from the tropics of America the are occasionally used for animal feed. In most cases, they are dis-
taste and its numerous health benefits made it popular in all the posed, producing phytopathogens that cause ecological problems
continents. Papaya is a tropical fruit having commercial importance and pose risks to human health [2].
because of its high nutritive and medicinal value. Papaya cultivation The food wastes/by-products can be a major pool of substances
had its origin in South Mexico and Costa Rica. Total annual world with very high potential to the pharmaceutical, food and cosmetics
production is estimated at 6 million tonnes of fruits. India leads manufacturing, while the development of processes for their (bio)-
the world in papaya production with an annual output of about 3 production and recovery would provide an irrefutable economic
million tonnes. Other leading producers are Brazil, Mexico, Nigeria, benefit for the agri-food sector and a direct, positive environmen-
Indonesia, China, Peru, Thailand and Philippines. tal impact [3,4]. From the extensive literature analysis, it was found
Papaya fruit is well-known worldwide for its benefit and flavor. that, no research report has been found on the microwave-assisted
Especially in India, the green fruit is widely used for cooking pur- extraction (MAE) of pectin from waste papaya (Carcia papaya L) peel
pose. Because of its high antioxidant content, papaya can prevent (WCPP). Therefore, the present study has been planned to investi-
cholesterol oxidation and can be use in preventative treatments gate and optimize the process parameters (microwave power, pH,
against atherosclerosis, strokes, heart attacks and diabetic heart time and solid-liquid ratio) on the maximum extraction of pectin
disease [1]. As the consumption and harvest increases, left are from WCPP by MAE method using four factors three levels Box-
large quantities of by-product papaya peels. There are many uses Behnken response surface design.
of papaya peel including as an ingredient in many skin and hair
care papaya products. The papaya peel can also be used in many 2. Materials and methods
home remedies. Application of the pulp or the peel with a little
milk and honey can help protect, soothe and moisturize the skin. In 2.1. Raw materials and reagents

Raw materials (WCPP) were obtained from local juice processing


∗ Corresponding author. Tel.: +91 4294 226606; fax: +91 4294 220087. stall near Perundurai, Erode, Tamilnadu, India. The peels were
E-mail address: prakashmaran@gmail.com (J.P. Maran). washed, manually cut and blanched for 5 min in boiling water. Then

http://dx.doi.org/10.1016/j.ijbiomac.2014.11.008
0141-8130/© 2014 Elsevier B.V. All rights reserved.
J.P. Maran, K.A. Prakash / International Journal of Biological Macromolecules 73 (2015) 202–206 203

Table 1
Experimental design matrix with observed and predicted values.

Std order Microwave power (w) pH Time (s) SL ratio (g/ml) Pectin yield (%)

1 480 (0) 2 (0) 180 (1) 5 (−1) 16.39


2 480 (0) 3 (1) 100 (0) 25 (1) 9.02
3 320 (−1) 2 (0) 180 (1) 15 (0) 16.71
4 480 (0) 3 (1) 180 (1) 15 (0) 16.71
5 480 (0) 3 (1) 20 (−1) 15 (0) 2.49
6 480 (0) 1 (−1) 180 (1) 15 (0) 13.29
7 640 (1) 1 (−1) 100 (0) 15 (0) 17.83
8 480 (0) 2 (0) 20 (−1) 25 (1) 9.02
9 480 (0) 2 (0) 100 (0) 15 (0) 24.69
10 480 (0) 3 (1) 100 (0) 5 (−1) 13.38
11 480 (0) 2 (0) 100 (0) 15 (0) 24.59
12 640 (1) 2 (0) 100 (0) 25 (1) 19.14
13 480 (0) 1 (−1) 20 (−1) 15 (0) 12.29
14 320 (−1) 1 (−1) 100 (0) 15 (0) 8.18
15 320 (−1) 2 (0) 100 (0) 25 (1) 9.83
16 320 (−1) 2 (0) 100 (0) 5 (−1) 9.86
17 640 (1) 3 (1) 100 (0) 15 (0) 11.58
18 480 (0) 1 (−1) 100 (0) 25 (1) 12.69
19 480 (0) 2 (0) 20 (−1) 5 (−1) 12.57
20 480 (0) 1 (−1) 100 (0) 5 (−1) 12.09
21 640 (1) 2 (0) 20 (−1) 15 (0) 16.49
22 320 (−1) 2 (0) 20 (−1) 15 (0) 4.74
23 640 (1) 2 (0) 100 (0) 5 (−1) 18.13
24 320 (−1) 3 (1) 100 (0) 15 (0) 7.62
25 640 (1) 2 (0) 180 (1) 15 (0) 22.48
26 480 (0) 2 (0) 180 (1) 25 (1) 18.97
27 480 (0) 2 (0) 100 (0) 15 (0) 24.63
28 480 (0) 2 (0) 100 (0) 15 (0) 24.67
29 480 (0) 2 (0) 100 (0) 15 (0) 24.64

the peels were dried at 50 ◦ C until it attains the constant weight. The the method illustrated by Maran et al. [7]. The experimental data
dried peels were grounded in order to obtain powdered sample and was analyzed by multiple regression analysis in order to develop an
it was stored in a dry environment prior to the experimental anal- empirical model, which exhibits the relationship between response
ysis. All solvents and chemicals used in this study were analytical and independent variables. Analysis of variance (ANOVA) was used
grade and purchased from Merck chemicals, Chennai, India. to analyze the effects of process variables statistically. The statis-
tical package Design- Expert 8.0.7.1 (State-Ease Inc., Minneapolis,
2.2. Microwave assisted extraction of pectin MN, USA) was used to construct the experimental design and anal-
ysis of experimental data.
A household microwave oven (LG, MH-3948 WB) at working
frequency of 2450 MHz with adjustable microwave power and irra- 3. Results and discussion
diation time was used to extract pectin from WCPP under different
extraction conditions (Table 1). After a selected time, the mixture in 3.1. Model fitting and statistical analysis
Pyrex beaker was cooled down to room temperature, filtered using
filter paper (Whatman no-1), centrifuged (5500 rpm for 15 min) The experimental data was analyzed by multiple regression
and the supernatant was precipitated with an equal volume of 95% analysis, fitted to various models (linear, interactive (2FI), quadratic
(v/v) ethanol. The coagulated pectin mass was washed with 95% and cubic) and the results showed that quadratic model incorpo-
(v/v) ethanol for three times and the wet pectin was subjected to rating linear, interactive and quadratic terms exhibited higher R2 ,
drying at 50 ◦ C in the hot air oven until it attains a constant weight. adjusted R2 , predicted R2 and also low p-values, when compared to
The pectin yield (PY) was calculated from the following equation other models. The relationship between independent variables and
proposed by Maran et al. [5]. response was exhibited by an empirical quadratic model developed
m  through multiple regression analysis of experimental data and the
0
PY = × 100 (1) final model acquired in terms of uncoded factors is given below
m
where m0 (g) is the weight of dried pectin and m (g) is the weight PY (%) = −91.81 + 0.24X1 + 33.32X2 + 0.15X3 + 1.5X4 − 8.8E
of dried waste papaya peel powder. − 003X1 X2 − 1.17E − 004X1 X3 + 1.63E − 004X1 X4

2.3. Experimental design + 0.04X2 X3 − 0.12X2 X4 + 1.92E − 003X3 X4 − 195E

− 003X12 − 8.16X22 − 7.87E − 004X32 − 0.052X42 (2)


Four factors (microwave power (X1 ), pH (X2 ), time (X3 ) and
solid–liquid (SL) ratio (X4 )) three level Box-Behnken response sur-
face design (Table 1) was employed in this study to investigate The observed data was analyzed by Pareto analysis of variance
and optimize the effect of process variables on the pectin yield (ANOVA) and the results were shown in Table 2. ANOVA of the
(response) from WCPP. The process variables range was selected regression model (Eq. (2)) showed that the developed quadratic
from the single-factor experimental results. The process variables model was highly significant, as was evident from the Fisher’s F-
were coded according to the method described by Prakash Maran test (F model = 82.40) with a very low probability value (<0.0001).
et al. [6]. A total of 29 experiments including 5 center points were The goodness of fit of the model was evaluated by the determi-
designed and the total number of experiments was calculated by nation co-efficient (R2 ), adjusted determination co-efficient (Ra2 ),
204 J.P. Maran, K.A. Prakash / International Journal of Biological Macromolecules 73 (2015) 202–206

Table 2
Analysis of variance of developed regression model for pectin yield.

Source Coefficient estimate Sum of squares Degree of freedom Mean square F value p-value

Model 24.64 1100.06 14 78.58 82.40 < 0.0001


X1 4.06 197.72 1 197.72 207.34 < 0.0001
X2 −1.30 20.20 1 20.20 21.18 0.0004
X3 3.91 183.69 1 183.69 192.63 < 0.0001
X4 −0.31 1.17 1 1.17 1.23 0.2863
X12 −1.42 8.09 1 8.09 8.49 0.0113
X13 −1.50 8.94 1 8.94 9.37 0.0084
X14 0.26 0.27 1 0.27 0.28 0.6027
X23 3.31 43.69 1 43.69 45.82 < 0.0001
X24 −1.24 6.15 1 6.15 6.45 0.0236
X34 1.53 9.39 1 9.39 9.85 0.0073
X1 2 −4.98 160.70 1 160.70 168.52 < 0.0001
X2 2 −8.15 431.37 1 431.37 452.35 < 0.0001
X3 2 −5.03 164.27 1 164.27 172.26 < 0.0001
X4 2 −5.16 173.04 1 173.04 181.45 < 0.0001

Fig. 1. Diagnostic plots for developed model adequacy.


J.P. Maran, K.A. Prakash / International Journal of Biological Macromolecules 73 (2015) 202–206 205

predicted determination co-efficient (Rp2 ) and co-efficient of vari- accord between the actual and predicted data’s. Normal distri-
ance (CV) and signal to noise ratio (S/N). In this study, the value of bution plot is used to analyze the distribution of the residuals.
determination coefficient (R2 = 0.988) indicated that only 0.12% of Residuals are the difference between the observed value and the
the total variations was not explained by the developed regression theoretically fitted value. The minimum the residual value the more
model. In addition, the value of adjusted determination coefficient meticulous the model prediction is [8,9]. If the residuals follow the
(Ra2 = 0.976) was also very high, indicating a high significance of straight line, it indicates that the residuals are distributed normally.
the model developed through experimental data. The value of Rp2 The normality assumption is analyzed by constructing a normal
(0.931) is in reasonable agreement with the value of Ra2 (0.976) and probability plot of residuals and it is given in Fig. 1b. The results
also shows that the form of the model chosen to explain the rela- apparently exhibits that there is no deviation of variance as the
tionship between the factors and the response is well-correlated. residuals were normally distributed. By constructing internally stu-
Furthermore, a very high degree of precision and a good deal of the dentized residuals versus experimental runs plot (Fig. 1c), a check
reliability of the conducted experiments were indicated by a low was made to analyze the experimental data and find out the satis-
value of the coefficient of variation (CV = 6.51%). Adequate preci- factory fit of the developed model [10,11]. As seen in Fig. 1c, all the
sion measures the signal-to-noise ratio and the ratio greater than data points lay within the limits (±2) and indicated the adequate
4 is desirable. In this study, the adequate precision was found to be fit of the developed model.
30.90, which indicates the best fitness of the developed model.
It is mandatory to affirm that the fitted model provide an ample 3.2. Three dimensional (3D) response surface and contour plots
approximation to the actual values in order to ignore the poor or
misleading effect on investigation and optimization (Maran et al., In order to visualize the relationship between the response
2012). The data points in the graph drawn between predicted and process factors, 3D response surface and contour plots were
versus actual values of this study found to be adjacently dispersed generated from the model equation (Eq. (2)) developed in this
(Fig. 1a). This indicates the minimum deviation and competent study, which could facilitate the straight forward examination of

Fig. 2. Influence of process variables on pectin yield.


206 J.P. Maran, K.A. Prakash / International Journal of Biological Macromolecules 73 (2015) 202–206

the effects of the experimental variables on the response [12,13]. optimal condition which could yield maximum pectin yield
From the Fig. 2, it was observed that, there was a perfect interac- (25.41%) was obtained as follows: microwave power of 512 w,
tion between the independent variables and response, which was pH of 1.8, time of 140 s and solid–liquid ratio of 1:15 g/ml respec-
confirmed by the smallest ellipse in 3D surface diagram and also tively. The suitability of the optimized conditions for predicting
elliptical contours in contour plots [14,15]. the optimum response values was tested experimentally using
The pectin yield was increased from 320 to 510 w by due to the selected optimal conditions. Triplicate experiments were per-
the heating principles of ionic conduction and dipole rotation of formed under the optimized conditions in order to find out the
MAE [16]. The electromagnetic energy was transferred rapidly on suitability of the optimized conditions to extract maximal pectin
the bio-molecules by ionic conduction and dipole rotations, which from WCPP. The mean values (25.39 ± 0.05) obtained from real
result more power was dissipated inside the solvent and plant experiments were well correlated with predicted values at optimal
materials which generate molecular movement and heating [17] condition.
on the extraction system rapidly and enhanced the loosening of
the cell wall matrix quickly, increases the penetration of the sol- 4. Conclusion
vent into the plant matrix which leads to enhanced the leaching of
pectin from plant material to solvent. The yield was decreased with In this study, four factors three level BBD was successfully
increasing the power beyond 510 w. used to investigate and optimize the process variables (microwave
From the results (Fig. 2), it was found that, the extraction yield power, pH, time and SL ratio) on the pectin yield from WCPP. From
of pectin was increased from the pH of 1–2. The low acidic sol- the results, it was observed that, all the process variables have sig-
vent has the ability to reduce the molecular weight of the pectin nificant effect on the extraction of pectin. The optimal condition
and increased the hydrolysis of insoluble pectin to soluble pectin which could yield maximum pectin yield (25.41%) was obtained
without any degradation in to the solvent [18]. Both these effects as follows: microwave power of 512 w, pH of 1.8, time of 140 s
contrarily influence the extraction yield of pectin [19]. The aggre- and solid–liquid ratio of 1:15 g/ml respectively and the real exper-
gation of pectin occurs beyond the pH value of 2, which retard the iments at optimal condition was well correlated with predicted
pectin release from plants and decreased the yield. values.
Fig. 2 Response surface plots showing the influence of process
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