Article

Microwave-assisted extraction for recovery

of polyphenolic antioxidants from ripe mango
(Mangifera indica L.) peel using lactic
acid/sodium acetate deep eutectic mixtures

Chandra Bhushan T Pal and Girirajsinh C Jadeja

Abstract
The present study investigates recovery of polyphenolic compounds from ripe mango (Mangifera indica L.)
peel using deep eutectic solvents based on microwave-assisted extraction method. Lactic acid/sodium acet-
ate/water (3:1:4) screened out from eight different types of deep eutectic solvent systems was used as
extractant. A Box–Behnken design along with response surface methodology was applied to optimize the
effect of microwave power (W), time (min), and liquid-to-solid ratio (mL g1) on polyphenol extraction. The
optimized conditions determined were power of 436.45 W, time of 19.66 min, and liquid-to-solid ratio of
59.82 mL g1. Under the optimal conditions, the recovery of total phenolic content, ferric reducing antioxidant
power, and 2,2-diphenyl-1-picrylhydrazyl scavenging activity was 56.17 mg gallic acid equivalent g1 dw,
683.27 mmol ascorbic acid equivalent g1 dw, and 82.64 DPPHsc%, respectively. High Performance Liquid
Chromatography (HPLC) analysis revealed mangiferin as the prominent phenolic compound in the mango
peel extracts. Microwave-assisted deep eutectic solvent extraction showed remarkable effects on the extrac-
tion efficiency of phenolic compounds as revealed from scanning electron microscopy analysis. Rancimat test
results revealed that the oxidative stability almost doubled upon addition of purified mango peel extracts to
the sunflower oil and thus paving way for the use of mango peel waste as a potential source of antioxidants.

Keywords
Antioxidant activity, mango peel, microwave-assisted deep eutectic solvent extraction, polyphenolic com-
pounds, Rancimat test, response surface methodology
Date received: 7 February 2019; accepted: 16 July 2019

bioconversion, recycling, and utilization of bioactive

INTRODUCTION
Globally, huge quantity of wastes is generated every
year by food processing industries, leading to a serious
environmental problem, but only a fraction of this is
recycled and reutilized via usage in the form of fertil-
izer, animal feed, etc. (Kasapidou et al., 2015; Kiran
et al., 2014). Due to this, there is a critical requirement
for adding value to these fruit and vegetable wastes. Of
late, many researchers are working on the recovery,
Food Science and Technology International 26(1) 78–92
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DOI: 10.1177/1082013219870010
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compounds from fruit waste (Galanakis, 2012; Roy
and Lingampeta, 2014). Usage of synthetic antioxi-
dants like butylated hydroxyl toluene and butylated
hydroxyl anisole as food additives is endangering
human health due to their toxicity and carcinogenicity.
Some European countries have banned these synthetic
antioxidants. Green consumerism resulting from
Chemical Engineering Department, S. V. National Institute of
Technology, Surat, India
Corresponding author:
Girirajsinh C Jadeja, Chemical Engineering Department, S. V.
National Institute of Technology, Dumas Road, Surat 395007,
Gujarat, India.
Email: jgc@ched.svnit.ac.in

enhanced health awareness and stringent governmental
regulations regarding use of synthetic chemicals has
paved way for naturally derived antioxidants not only
in food industry but also in medicinal applications.
Mango is ranked third among the various tropical
fruits produced. Recent data from the Food and
Agriculture Organization of the United Nations
(2017) declared India as the topmost producer of
mango, with production of over 18 million tons in
2017 accounting for nearly 50% of the global mango
supply. Gujarat and Maharashtra states in India pro-
duce around 1.99 million tons of mangos (Department
of Agriculture, Cooperation & Farmers Welfare, 2016).
Major varieties of mango grown in India
include Alphonso, Banganapalli, Chausa, Dashehari,
Jamadar, Kesar, Neelum, Suvarnarekha, Totapuri,
Rajapuri, and Langra (Agricultural & Processed Food
Products Export Development Authority, 2017).
Valuable antioxidants are found in the parts of
mango plant such as peel, seed kernel, bark, leaves,
and pulp which are used in the biomedical applications
including free radical scavenging (Ajila et al., 2007a;
Ribeiro et al., 2007), anti-inflammatory (Hernandez
et al., 2007) and anticancer activities (Percival et al.,
2006). Mango peel is the main by-product obtained
from the pulp processing industries. It constitutes
about 15–20% of the fruit weight. Nowadays, peel
and kernel are discarded as waste after pulp extraction
from fruit and constitute an important source of pollu-
tion (Ajila et al., 2007b). Peel is a rich source of poly-
phenols, fiber, carotenoids, vitamin E, and vitamin C
(Ajila et al., 2007a) and it exhibited good antioxidant
properties (Ajila et al., 2007b). Lakshminarayana et al.
(1979) reported that the polyphenolic content in peel
was greater than that of flesh.
Food industries recover valuable bioactive compounds
from natural sources using different extraction tech-
niques. Extraction is the primary footstep for the revival
and refinement of precious polyphenolic compounds
from plant matrix. Major conventional techniques
being employed like Soxhlet extraction, heating–stirring
method, heat-refluxing, etc. consume large quantity of
solvents and require longer extraction time. Compared
to traditional techniques, microwave-assisted extraction
(MAE) has few important merits with reduced solvent
consumption, shorter extraction time, automated tech-
niques, and increased pollution prevention concern (Cui
et al., 2015; Cvjetko Bubalo et al., 2016).
Deep eutectic solvents (DESs) are known as green
solvents because of their properties such as nontoxicity,
inexpensive, absence of flammability, negligible vapor
pressure, recyclable, and environmentally friendly (Cui
et al., 2015). DESs have unique potency to give higher
yield in extraction of natural products than those
obtained using traditional techniques. Considering the
Pal and Jadeja
above concepts and perspectives, microwave-assisted
deep eutectic solvent extraction (MADESE) was used
to extract the major bioactive compounds from ripe
mango peels. In total, eight types of DESs were used
in this study. DES system consisting of lactic acid/
sodium acetate (LA:SA) provided the best outcome
for total phenolic content (TPC) from mango peel.
This mixture was used further to determine TPC and
antioxidant activities such as ferric reducing antioxi-
dant power (FRAP) and 2,2-diphenyl-1-picrylhydrazyl
(DPPH) radical scavenging activities. A Box–Behnken
design (BBD) along with response surface methodology
(RSM) was applied to optimize the effect of microwave
power (W), time (min), and liquid-to-solid ratio
(mL g1) on polyphenol extraction. BBD has been
widely applied to optimize the extraction of bioactive
compounds from various natural sources (Cui et al.,
2015; Das and Mandal, 2015; Fattahi and Rahimi,
2016; Maran et al., 2013; Shirzad et al., 2017).
The aim of this study was to determine the optimal
conditions for the extraction of phenolic compounds
(PCs) from mango peel by MADESE using LA:SA
mixtures. Rancimat method was used to check the
effect of extract on the oxidative stability of sunflower
oil. Scanning electron microscopy (SEM) analysis was
also conducted to study the impact of microwave
irradiations on the peel during extraction.
MATERIAL AND METHODS
Chemicals and reagents
Analytical standard mangiferin (99.0%) was procured
from Sigma-Aldrich, Germany. Ferric chloride (FeCl3)
(anhydrous) and ascorbic acid were from Rankem
Laboratory, Thane. Folin–Ciocalteu reagent, gallic
acid, sodium carbonate (Na2CO3), DPPH, and 2,4,6-
trippyridyl-s-triazine were supplied by Sisco Research
Laboratories Pvt. Ltd., Taloja, Maharashtra.
Chloroform, methanol, hydrochloride acid, urea, sorb-
itol, sucrose, glycerol, lactic acid, malic acid, choline
chloride, and sodium acetate were purchased from
Finar Ltd, Ahmedabad. Distilled water was used for
HPLC analysis.
Plant material
Ripe mangoes (Kesar variety) used in this study were
purchased from a local market of Valsad, India.
Removal of peel was carried out manually by knife
and pulp was scrapped with its blunt edge. The
mango peels were dried using an oven at 60  C until it
attained constant weight. The dried peel was powdered
in a high-speed mixer (Blender 7012S; Waring,
Torrington, CT, USA) and screened using 210 mm
B.S.S 72 sieve (Kumar Test sieves, Mumbai).
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Food Science and Technology International 26(1)

The powder was kept in a zip lock polybag and stored Table 1. Details of the different DES systems used.
in desiccator till the extraction studies were carried out.
Abbreviation HBA HBD Mole ratio

DES-1 Choline chloride Urea 1:2

Preparation of DESs
DES-2 Choline chloride Sorbitol 3:1
The conditions used for preparation of DESs were as DES-3 Choline chloride Sucrose 1:1
per previously reported methodologies (Dai et al., 2015; DES-4 Choline chloride Glycerol 1:3
Mouratoglou et al., 2016). In this investigation, eight DES-5 Sodium acetate Glycerol 1:3
different types of DESs were prepared for obtaining
DES-6 Choline chloride Lactic acid 1:3
bioactive compounds from ripe mango peel (Table 1).
DES-7 Sodium acetate Lactic acid 1:1, 1:2,
DESs were prepared using heating and stirring method
1:3, 1:4
under suitable condition of temperature 70  C, 600 rpm,
DES-8 Choline chloride Malic acid 1.5:1
and 60–120 min time.
DES: deep eutectic solvent; HBA: hydrogen bond acceptor; HBD:
hydrogen bond donor.
Extraction methods
Heating–stirring extraction (HSE). Appropriate quan- which 1 g peel powder was added and the mixture was
tity of mango peel powder was taken into a beaker stirred at 500 rpm for 120 min. The slurry was Eltered
with different DES systems (Table 1) which was through Elter paper (Whatman No. 1) followed by ana-
placed on a magnetic stirrer at 500 rpm, 60  C for lysis of the extracts to evaluate the TPC using the
90 min. Liquid-to-solid ratio was maintained at 50:1 Folin–Ciocalteu method.
(mL g1) for each sample. Samples were filtered
through Whatman paper No. 1 after the completion
Measurement of TPC
of each extraction and the resulting clear supernatant
was used for TPC analysis. The TPC of mango peels from DES extracts was
determined using Folin–Ciocalteu method (Singleton
MAE. LA:SA eutectic mixture (DES-7) resulted in the and Rossi, 1965). UV-spectrophotometer (HACH
highest TPC by HSE. Therefore, this solvent was con- DR-6000) was used to read absorbance at 760 nm
sidered for further studies to optimize the extraction of and the total phenolics in each extract was calculated
PCs employing microwave radiations and subsequent from a calibration curve (Y ¼ 0.0005x; R2 ¼ 0.993),
antioxidant assays. A modified domestic microwave using gallic acid as a standard (25–500 mg l1). The
oven (Samsung, Seremban, Malaysia) was used for results were determined as mg gallic acid equivalent
the extraction purpose (Thakker et al., 2016). The (GAE) g1 dw.
apparatus was equipped with a digital control system
for measuring irradiation time and power. The oven
Antioxidant assays
has an output power range of 100–800 W (230–240 V,
50 Hz) with an operating frequency of 2450 MHz. The FRAP assay. Benzie and Strain (1996) developed meth-
oven was modified by making a hole at the top to odology to determine ferric reducing ability of mango
accommodate the reflux condenser. Appropriate quan- peel extracts. Calibration curve was prepared of ascor-
tity of mango peel powder was taken in a round bottom bic acid (30–220 mmol). The reducing power of the
flask (250 mL) with certain volume of DES added to it. extracts was determined from the standard curve
The flask was then placed in the central position of (Y ¼ 0.001 x; R2 ¼ 0.995) and the results were repre-
microwave oven and subsequently subjected to different sented in the form of mmol ascorbic acid equivalent
combinations of microwave power (300, 450, 600 W), (AAE) g1 dw. An absorbance of each extract was rec-
irradiation time (15, 20, 25 min), and liquid-to-solid orded at 620 nm using UV-spectrophotometer (HACH
ratio (40:1, 50:1, 60:1 mL g1) as per Box–Behnken DR-6000).
experimental design. After extraction, the flask was
allowed to cool before collecting the extracts. The DPPH assay. The radical scavenging activity of mango
resulting extracts were filtered using filter paper peel extracts was determined using previously reported
(Whatman No. 1) and subsequently analyzed. protocol (Brand-Williams et al., 1995). Briefly,
0.985 mg DPPH was diluted with 25 mL of methanol
Conventional extraction. Traditional solvent extrac- and prepared 100 mM solutions. Now, 0.025 mL of
tion method was also implemented to extract the PCs extracts was taken in a test tube and 0.975 mL of
from mango peels for comparative analysis. Fifty milli- DPPH solution added and shaken properly. The
liters of 70% aqueous ethanol was taken in a beaker to sample was kept in dark for 30 min. After this

80

procedure, the absorbance was recorded at 515 nm
using UV-spectrophotometer (HACH DR-6000).
Equation (1) estimates the inhibition of free radicals
by the extract
 
Ac  As
Ið%Þ ¼  100 ð1Þ
Ac
where Ac ¼ Absorbance of DPPH solution,
As ¼ Absorbance of DPPH along with different con-
centrations of test samples
Recovery of mangiferin after DES extraction
using liquid–liquid extraction
A previously published methodology was used with
slight modification (Pal and Jadeja, 2019). In this
work instead of ethyl acetate, chloroform was found
to be more effective and hence employed as an aprotic
solvent for recovering mangiferin from the DES
extracts.
HPLC analysis
The HPLC analysis was carried out with respect to the
method reported by Makasana et al. (2017). PCs in the
deep eutectic extract made of LA:SA were separated in
C18 chromatographic column with column temperature
at 40  C using HPLC system (Shimadzu Corporation,
Kyoto, Japan) equipped with UV–Vis detector (model
SPD-20 A), a degasser (model DGU-20A3), a quater-
nary pump (model LC-20AD), a column oven (model
CTO-10ASvp), and an auto sampler (model SIL-
20ACHT) connected to CBM-20 communication bus
module system. The mobile phase consisted of isocratic
acetonitrile (45%) and 0.1% formic acid in water
(55%). The results were achieved by comparison of
peak areas of the crude samples with that of standards.
The peaks were detected at wavelength of 370 nm using
UV absorbance with flow rate 1.0 mL min1 for a total
run time of 20 min.
Rancimat assay for oxidation stability of oil
Rancimat test was used to evaluate the oxidative sta-
bility of oil by measuring the length of the induction
time. 37.5 mg of extracts was dissolved in 1 mL metha-
nol and the resulting solution was added to 10 g sun-
flower oil under ultrasonic treatment (ElmaÕ
Transsonic TI-H-5, Germany) at 25 kHz frequency,
100 W power for 15 min. Oxidative stability was deter-
mined using Rancimat tubes containing 2 g of each
mixture. Experiments were performed at 120  C for
20 h using Rancimat (Metrohm, Switzerland)
Pal and Jadeja
instrument (Sun and Ho, 2005; Taha et al., 2010). Air
supply was maintained at 20 l h1.
Morphological description of mango peels after
extraction
Microstructure analysis of fresh mango peel and resi-
dual mango peel with different extraction methods was
examined by SEM. The samples were coated using gold
alloy with double sided adhesive tape and imaged in a
SEM device (Hitachi Series 3400N).
RSM
Three factors and three levels were selected for BBD
and 17 runs with five center points were employed in
this study (Das and Mandal, 2015; Maran et al., 2013).
Three major independent factors such as microwave
power (A), time (B), and liquid-to-solid ratio (C) were
chosen and coded at three levels by associating signs
(1, 0, þ1) for lower, center, and higher levels, respect-
ively. Table 2 shows the experimental design matrix and
levels. Second-order polynomial model (equation (2))
was used for fitting the experimental results and mul-
tiple linear regressions provided the coefficients
X
3 X
3 X
3
Yn ¼ b 0 þ b i Xi þ bii Xij þ bij Xi Xj ð2Þ
i¼1 i¼1 i6¼j¼1
where (Yn) represents the responses TPC, FRAP, and
DPPHsc% which are predicted for X1–X3; b0 repre-
sents the constant coefficient; b1, b2, and b3 are the
linear coefficients; b11, b22, and b33 show the quadratic
coefficients; and b12, b13, and b23 are the cross-coeffi-
cients (Fattahi and Rahimi, 2016).
Design Expert software v.10 provided the optimal
extraction condition using the desirability function.
Relationship among the response and the variables was
also presented by three-dimensional (3D) surface plots.
Statistical analysis
Response surface analysis was performed using the
Design Expert 10.0.8 software (Stat-Ease, Inc.,
Minneapolis, MN, USA). All experimental results are
the average of triplicate runs expressed as
mean  standard deviation.
RESULTS AND DISCUSSION
DES screening for extraction of mango
peel PCs
In the present investigation, eight types of DESs were
used for the extraction of PCs from mango peels. DESs
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Food Science and Technology International 26(1)

Table 2. Box–Behnken design with experimental and predicted values of TPC, FRAP, and DPPHsc%.

Factors Experimental Predicted (RSM)

Run A B C TPC FRAP DPPHsc% TPC FRAP DPPHsc%

1 0 0 0 40.46 695.22 81.99 40.59 696.16 81.57

2 0 1 1 36.12 445.44 80.35 35.94 453.48 80.39
3 1 0 1 56.17 630.22 82.45 55.67 623.49 82.59
4 1 1 0 37.54 653.40 81.49 37.22 638.62 81.59
5 1 0 1 55.36 632.25 82.58 55.62 642.34 82.54
6 0 1 1 54.98 643.43 82.16 55.04 648.12 82.10
7 1 0 1 35.12 440.26 80.15 34.86 430.17 80.19
8 1 1 0 36.14 588.54 80.25 36.46 603.32 80.15
9 1 0 1 36.44 441.36 79.98 36.94 448.09 79.84
10 0 0 0 40.98 698.27 81.15 40.59 696.16 81.57
11 0 1 1 35.62 442.12 77.85 35.56 437.43 77.91
12 0 0 0 39.45 695.55 81.48 40.59 696.16 81.57
13 0 0 0 41.64 701.37 81.65 40.59 696.16 81.57
14 1 1 0 39.08 592.64 81.25 39.52 594.68 81.17
15 0 1 1 55.78 638.40 81.35 55.96 630.35 81.31
16 0 0 0 40.41 690.38 81.57 40.59 696.16 81.57
17 1 1 0 41.24 598.21 79.25 40.80 596.16 79.33
Coded levels
Variables Symbols 1 0 1

Microwave power (W) A 300 450 600

Time (min) B 15 20 25
Liquid-to-solid ratio (mL g1) C 40 50 60
DPPHsc%: 2,2-diphenyl-1-picrylhydrazyl scavenging assay; FRAP: ferric reducing antioxidant power; RSM: response surface method-
ology; TPC: total phenolic content.

possess notable properties such as surface tension, vis-
cosity, density, polarity, and solubility which have
major impact on the extraction efficiency (Dai et al.,
2015). DES-7 (LA:SA) gave the best result among all
DESs (Figure 1(a)).Therefore, it was chosen as the
desired solvent for the subsequent extraction of phen-
olics from mango peel. The extraction efficiency of
DESs depends largely on their polarity, which in turn
is directly related to their solubilizing capacity.
However, detailed information regarding polarity of
DES is particularly limited (Tang and Row, 2013)
and thus only claims could be made regarding the
data obtained. Bakirtzi et al. (2016) proposed that poly-
phenols can be considered as a type of hydrogen bond
donor (HBD) and showed that there was a stronger
interaction of acetate anions with polyphenols leading
to their higher solubility and better extraction efficiency.
Effect of water content in DES
Figure 1(b) shows the effect of water content (0–100%
(v/v)) in LA:SA DES system to extract the TPC. It can
be seen that the highest TPC was achieved when water
addition was 30% (v/v). Hence, addition of water could
reduce the viscosity and surface tension substantially
(Cui et al., 2015; Dai et al., 2015; Ren et al., 2015).
Polarity is a further significant characteristic that
affects the solubilizing capacity of DESs.
Higher water content in LA:SA could reduce viscos-
ity of LA:SA and boost the polarity of the solvent.
However, extreme water in LA:SA could diminish the
hydrogen bond interconnection between LA:SA and
desired compounds resulting in the decline in extraction
yield of the desired compounds (Dai et al., 2015; Peng
et al., 2016). Therefore, 30% (v/v) water in LA:SA mix-
ture was employed in further experiments for optimiza-
tion of various factors such as microwave power, time,
and liquid-to-solid ratio.
Effect of molar ratio in DES
Molar ratio of DESs plays a critical role on the extrac-
tion efficiency (Cui et al., 2015). In this study, LA:SA
having different molar ratios was used for the

82
 Pal and Jadeja

Experiments were performed in triplicates for the inde-

(a)
TPC (mg GAE g–1 dw) 100 pendent variables: A (microwave power, W), B (time,
80 min), and C (liquid-to-solid ratio, mL g1). Table 3
60 shows the ANOVA results for the RSM model which
40
indicates that the p values < 0.01 were considered to be
significantly accurate for each of the three responses. In
20
this study, the value of regression coefficients, R2 and
0
DES-1 DES-2 DES-3 DES-4 DES-5 DES-6 DES-7 DES-8
R2-adj, for TPC, FRAP, and DPPHsc% was > 0.98
Deep eutectic solvent systems
and 0.96, which recommends the fitness of the RSM.
(b) Regarding lack of fit in the RSM model, TPC and
80
DPPHsc% responses were insignificant as p > 0.05
TPC (mg GAE g–1 dw)

60 while FRAP was significant (0.0084), indicating that

40
the model fits well and there is significant effect of par-
ameter on output response (Puertolas et al., 2011).
20 Though the lack of fit for the FRAP model was signifi-
0
cant, the adjusted R2 (0.9855) was very close to the R2
0% 10% 30% 50% 70% 90% 100% value (0.9936), indicating that even after removing
Water content (% v/v) some terms, the quality of the model was maintained.
(c)
100 Table S1 shows the relative errors of FRAP which
TPC (mg GAE g–1 dw)

80 measure the percentage of deviation between the experi-

60
40
20
0 (Arruda et al., 2017).
1:1:4
Molar ratio of lactic acid/Sodium acetate/Water
Figure 1. Effect of different DES systems (a), water con-
tent in DESs (b), and LA:SA molar ratio (c) on TPC. DES:
deep eutectic solvent; GAE: gallic acid equivalent; TPC:
total phenolic content.
extraction of TPC (Figure 1(c)). TPC initially increased
with an increase in molar ratio of LA:SA/water from
1:1:4 to 3:1:4 (mol/mol/mol), and then decreased for
molar ratio 4:1:4. This is due to the amount of lactic
acid (HBD) being excess in eutectic mixture which is
responsible for viscosity. Therefore, as mole of lactic
acid increases, viscosity of the eutectic mixture also
increased. Therefore, after a certain molar ratio, extrac-
tion yield decreases due to higher viscosity (Cui et al.,
2015). It was due to a decrease in the quantity of
sodium acetate compared to HBD lactic acid, which is
attributed to the reduction of proportion of hydrogen
bond acceptors in the DESs. Wei et al. (2015) also
reported similar type of results. Considering the above
results, LA:SA/water with a molar ratio 3:1:4 (mol/mol/
mol) was selected for the subsequent experiments.
Optimization of extraction parameters and
model fitting
Table 2 shows the BBD along with experimental and
predicted values of TPC, FRAP, and DPPHsc%.
mental and model predicted values. Relative errors are
found to be very low for all the runs, which show that
the quality of the model is fit to the experimental values
2:1:4 3:1:4 4:1:4
Liquid-to-solid ratio (p < 0.01) was influenced on
linear terms of TPC, FRAP, and DPPHsc%. In add-
ition, another important variable, time (p < 0.01) also
has an effect on DPPHsc%. Interaction effects of the
independent variables AB were highly significant in the
case of TPC and AB was marginally significant on
FRAP while AB and BC were significant on
DPPHsc%. The quadratic terms of A2 and B2 were
significant while C2 was highly significant in the case
of TPC. In the case of FRAP, all three quadratic terms
were highly significant. The quadratic terms of B2 were
very powerful for DPPHsc% while rest of the terms
were insignificant because their p value was greater
than 0.05. It is conflicting to the other responses
which prove to be statistically highly powerful
(p < 0.01). If the values are greater than 0.1, model
terms are not significant. On the above discussion, it
can be seen that the lower p value and higher R2 have
higher significant effect on the respective response vari-
ables (Fattahi and Rahimi, 2016).
Experimental data by RSM models for each of
the responses are expressed on the basis of equa-
tions (3) to (5)
YTPC ¼ 114:03550  0:061935A þ 2:48590B
 5:45713C þ 2:21333  103 AB  3:5500
 104 AC þ 6:50  103 BC þ 4:31222
 105 A2  0:04471B2 þ 0:061548C2
ð3Þ

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Food Science and Technology International 26(1)

Table 3. ANOVA analysis for the responses of TPC, FRAP, and DPPHsc%.
Source Sum of squares df Mean square F value p-value Prob > F

TPC
Model 958.90 9 106.54 190.96 <0.0001 Significant
A-Power 2.07 1 2.07 3.71 0.0954
B-Time 0.14 1 0.14 0.25 0.6313
C-L/S ratio 779.93 1 779.93 1397.88 <0.0001
AB 11.02 1 11.02 19.76 0.0030
AC 1.13 1 1.13 2.03 0.1970
BC 0.42 1 0.42 0.76 0.4130
A2 3.96 1 3.96 7.10 0.0322
B2 5.26 1 5.26 9.43 0.0181
C2 159.50 1 159.50 285.87 <0.0001
Residual 3.91 7 0.56
Lack of fit 1.30 3 0.43 0.67 0.6150 Not significant
Pure error 2.60 4 0.65
R2 ¼ 0.9959
Adj R2 ¼0.9907
FRAP
Model 1.531105 9 17,014.27 121.62 <0.0001 Significant
A-Power 676.38 1 676.38 4.83 0.0638
B-Time 571.90 1 571.90 4.09 0.0829
C-L/S ratio 75,101.38 1 75,101.38 536.83 <0.0001
AB 652.55 1 652.55 4.66 0.0676
AC 0.22 1 0.22 1.546103 0.9697
BC 0.73 1 0.73 5.225103 0.9444
A2 9357.64 1 9357.64 66.89 <0.0001
B2 7015.11 1 7015.11 50.14 0.0002
C2 53,757.31 1 53,757.31 384.26 <0.0001
Residual 979.29 7 139.90
Lack of fit 913.03 3 304.34 18.37 0.0084 Significant
Pure error 66.26 4 16.57
R2 ¼0.9936
Adj R2 ¼0.9855
DPPH
Model 23.63 9 2.63 40.51 <0.0001 Significant
A-Power 0.080 1 0.080 1.23 0.3033
B-Time 5.36 1 5.36 82.74 <0.0001
C-L/S ratio 13.03 1 13.03 201.04 <0.0001
AB 0.38 1 0.38 5.93 0.0451
AC 0.023 1 0.023 0.35 0.5742
BC 0.71 1 0.71 11.02 0.0128
A2 0.022 1 0.022 0.34 0.5760
B2 3.68 1 3.68 56.82 0.0001
C2 0.18 1 0.18 2.74 0.1420
Residual 0.45 7 0.065
Lack of fit 0.086 3 0.029 0.31 0.8159 Not significant
Pure error 0.37 4 0.092
R2 ¼ 0.9812
Adj R2 ¼ 0.9569

ANOVA: analysis of variance; DPPH: 2,2-diphenyl-1-picrylhydrazyl; DPPHsc%: 2,2-diphenyl-1-picrylhydrazyl scavenging assay; FRAP:
ferric reducing antioxidant power; TPC: total phenolic content.

84

YFRAP ¼ 3487:842 þ 1:49156A þ 56:3814B
þ 122:9225C þ 0:017030AB  1:55
 104 AC  8:55  103 BC  2:09523
 103 A2  1:63271B2  1:12993C2
ð4Þ
YDPPHsc % ¼ 68:45675  2:190  103 A þ 0:72415B
þ 0:18638C þ 4:1333  104 AB  5:0
 105 AC þ 8:45  103 BC  3:2333
 106 A2  0:037410B2  2:0525  103 C2
ð5Þ
Y indicates the predicting responses and A, B, and C
represent microwave power, time, and liquid-to-solid
ratio, respectively.
Effects of extraction conditions on the TPC
based on RSM
As can be seen in Table 3, the terms C and C2 are highly
significant, while the terms AB, A2, and B2 are moder-
ately significant. The 3D surface plots described in
Figure 2(a) to (c) represent interaction between vari-
ables A to C for TPC. Prakash et al. (2007) have sug-
gested that contour plots can easily explain the nature
and extent of the interaction of various components.
The interactions between microwave power (A) and
time (B) are presented in Figure 2(a). A marginally sig-
nificant effect was observed in the interactions between
microwave power (A) and time (B) on the TPC
(Figure 2(a)).
As shown in Figure 2(b), liquid-to-solid ratio (C) was
another important independent parameter used for
extraction of PCs from mango peels. Initially, the extrac-
tion efficiency was very insignificant in the range of liquid-
to-solid ratio (40–50 mL g1) but when microwave power
rises with respect to liquid-to-solid ratio, high extraction
efficiency is obtained. When a higher liquid-to-solid ratio
is used in the extraction operation, concentration gradient
achieved was higher between the liquid and solid, result-
ing in an increase in the diffusion rate. In the absence of
adequate solvent, the diffusion rate decreases leading to
lower extraction efficiency (Katsampa et al., 2015). An
accurate liquid-to-solid ratio is very important for plenti-
ful mixing and maximum diffusion rate of the solute
resulting in enhanced extraction yield (Cacace and
Mazza, 2003). The highest TPC 54.98–56.17 mg GAE
g1 dw was achieved in the range of liquid-to-solid
ratio (58–60 mL g1) and microwave power (420–
600 W). There was significant effect of time on TPC in
the middle range (18–23 min) (Figure 2(c)). Prolonged
Pal and Jadeja
time might lead to degradation of polyphenolic com-
pounds and thereby lowering the TPC value.
FRAP
Figure 2(d) to (f) represents 3D surface plots of FRAP
which explain the interaction between variables A to C.
For reducing power, C, A2, B2, and C2 were highly
significant; A, B, and AB were marginally significant
while rest of the variables were insignificant on the
model terms. From Figure 2(d), it can be seen that
the maximum reducing power was obtained in the
microwave power range of 420–450 W for 17–21 min.
Extraction recovery rate increased by enhancing the
liquid-to-solid ratio but it subsequently decreased
when the microwave power was increased up to
480 W. The higher reducing power was determined
between 420 and 480 W and liquid-to-solid ratio of
52–60 mL g1 (Figure 2(e)). The cause for the stability
of reducing power activity can be attributed to the for-
mation of products of Maillard reaction. It was
reported that after heating there was an increase in
reducing power due to alteration in PCs (Tsai and
She, 2006). Under optimal conditions, the maximum
reducing power activity of 683.27 mmol AAE g1 dw
was obtained. The higher FRAP was observed in the
middle range of time (Figure 2(f)).
DPPH scavenging assay (DPPHsc%)
The 3D surface plots of DPPHsc% are shown in
Figure 2(g) to (i). For DPPH radical scavenging activity,
B, C, and B2 were highly significant; AB and BC were
significant while rest of the model terms were insignifi-
cant. According to Figure 2(g), it can be seen that within
420–450 W microwave power, the DPPHsc% value rises
with the increase in time (B). Initially, the DPPHsc%
value was very low in the range of time (15–21 min)
but when the microwave power increased with respect
to time, high DPPHsc% value was obtained. Increase in
microwave power with respect to time increases the TPC
of mango peel extracts and subsequently enhances
DPPHsc%. This is due to the dependency of antioxidant
activity on polyphenol concentration of the extracts to a
certain degree (Mouratoglou et al., 2016). Similar find-
ings were also observed for different agri-food waste
extracts (Makris et al., 2007). Maximum DPPHsc%
value was observed in the time range (21–23 min) but
beyond 23 min, the DPPHsc% value decreased with
respect to high microwave power due to degradation
of polyphenolic compounds. Liquid-to-solid ratio was
marginally significant in the range of 40–55 mL g1
while highly significant in the range of 55–60 mL g1
with microwave power of 420–480 W (Figure 2(h)).
Antioxidant values were improved by increasing both
85
Food Science and Technology International 26(1)

(a) (b) (c)

60 60

55 55

60 50 50

55 45 45

TPC
50 40 40

TPC
45 35 35
30
TPC

40 30

35
30
60 600 60 25
55 540 55 23
480 21
50 50
420 19
25 600 C: L/S ratio (mL/g) 45
540
C: L/S ratio (mL/g) 45 360 A: Power (W) 17 B: Time (min)
23 40 300 40 15
21 480
19 420
B: Time (min) 17 360 A: Power (W)
15 300

(d) (e) (f)

800
800 800
700
700 700
600 600 600
FRAP

FRAP

FRAP
500 500 500
400 400 400
600 25
25 60 540 60 23
600
23 55 480 55 21
540
21 50 420
480 50 19
19 420 A: Power (W) B: Time (min)
45 360 45 17
B: Time (min) 17 360 C: L/S ratio (mL/g) C: L/S ratio (mL/g)
A: Power (W) 40 300 40 15
15 300

(g) (h) (i)

83 83 83
82 82 82
81 81 81
DPPHsc%

80
DPPHsc%

80
DPPHsc%

80
79 79 79
78 78 78
77 77 77

600 25
25 60
600 60
540 23
23 540 55 55
480 21
21 480 50 420 50 19
19 420
45 360 A: Power (W) 45 17 B: Time (min)
B: Time (min) 17 360 A: Power (W) C: L/S ratio (mL/g) C: L/S ratio (mL/g)
40 300 40 15
15 300

Figure 2. The effect of three main factors on response variables based on their interactions: TPC (a–c); FRAP (d–f), and
DPPHsc% (g–i). DPPHsc%: 2,2-diphenyl-1-picrylhydrazyl scavenging assay; FRAP: ferric reducing antioxidant power;
TPC: total phenolic content.

Optimization of process variables for

parameters: microwave power and liquid-to-solid ratio.
responses
Higher liquid-to-solid ratio results in rise in mass trans-
fer which eventually leads to increase in TPC, FRAP, Optimization of three main responses, specifically,
and DPPHsc%. The peculiar effect was observed in the TPC, FRAP, and DPPHsc%, was determined using
interaction between time (B) and liquid-to-solid ratio (C) desirability values. Design Expert software gives the
on the DPPH scavenging (DPPHsc%). The highest desirability values of more than 0.97 under the opti-
DPPHsc% value (80–82.54%) was obtained in the mum condition as given in the Electronic supplemen-
range of time (19–23 min) and liquid-to-solid ratio tary material Figure S1. At the optimal conditions of
(56–60 mL g1) (Figure 2(i)). In the pharmaceutical, cos- microwave power of 436.45 W, irradiation time of
metic, and food industries, there is a crucial demand for 19.66 min, and liquid-to-solid ratio of 59.82 mg l1
antioxidant-rich extracts (Khiari et al., 2009). (Electronic supplementary material Figure S2), TPC,

86

FRAP, and DPPHsc% values obtained were 56.17 mg
GAE g1 dw, 683.26 mmol AAE g1 dw, and 82.54
DPPHsc%, respectively, and these data were very
close to the experimental values performed under opti-
mized conditions. In order to validate these results, the
experiments were performed at optimized conditions in
duplicates and values were averaged. Results obtained
were 55.28 mg GAE g1 dw for TPC, 680.55 mmol AAE
g1 dw for FRAP, and 82.64 for DPPHsc%.
Comparison of extraction methods
The proposed MADESE method was found to be an
efficient one in recovering phenolic antioxidants. The
free radical scavenging activity was reported to be
82.64% vis-à-vis 80.13% in case of extracts obtained
by employing traditional extraction. Moreover,
MADESE is six times faster than the conventional
extraction. The results obtained herein are well within
the range reported in previous studies. Rojas et al.
(2018) determined the TPC of Ataulfo variety mango
peel with ethanol solvent and found it to be 72.61 mg
g1. Umamahesh et al. (2016) studied five varieties of
mango, viz. Alphonso, Malgua, Rumani, Sindhura,
and Banisha for antioxidant activity. They found
Sindhura had higher TPC of 87.38  0.43 mg GAE
g1 dw. Sogi et al. (2013) reported TPC of 3185 mg
GAE 100 g1 db in case of freeze dried mango (cv
Tommy Atkins) peels. Tunchaiyaphum et al. (2013)
obtained TPC of 25.13 mg GAE g1 dw in Phalun
type mango peel using 95% ethanol as solvent in 4 h
Soxhlet extraction whereas subcritical water extraction
at 180  C for 90 min resulted in TPC of 30.62 mg GAE
g1 dw. Ajila et al. (2010) also investigated TPC of
Badami mango peels employing 80% acetone as solvent
and found it to be 54.67  1.5 mg g1. Free radical
scavenging activity in our studies (82.64%) was well
within the reported range of 79.6% (Ajila et al., 2008)
to 93.89% (Ashoush and Gadallah, 2011).
Identification and quantification of mangiferin
by HPLC
The mango peel extract obtained by conventional
method contained 1.0848 mg g1 mangiferin as com-
pared to 0.9301 mg g1 in MADESE extract.
Figure 3(a) and (b) shows the chromatograms of stand-
ard mangiferin and that of purified DES extract. DES
exhibits an important solvation property which is
robustly affected by hydrogen bonding. In this study,
chloroform was used to recover mangiferin from DES
extract. The mass transfer will take place among DES
droplets and nearby aprotic solvents. Partition coeffi-
cient plays a key role in the separation of PCs between
dispersed phase and aprotic solvents (Liu et al., 2016).
Pal and Jadeja
Mangiferin was the predominant compound in the cul-
tivars Chok Anan, Tommy Atkins, Maha Chanock,
and Kaew, with the contents ranging from 0.30 to
1.30 mg g1 on a dry matter basis (Berardini et al.,
2005). Our results are well within the reported range.
SEM
The SEM analysis was performed to determine the
shape and morphology of the fresh mango peel
powder as well as MADESE-treated residual samples.
Figure 4 shows the clear micro-mechanism changes in
the sample resulting from various extraction methods.
The microstructure of the plant material was slightly
ruptured during the HSE (Figure 4(b)). This is because
the heat transfer was generally executed with conduc-
tion and convection which have significant effect on the
disruption of raw materials. Consequently, the PCs
were extracted by solubilization and permeation.
However, SEM of the plant materials after MADESE
(Figure 4(c)) indicates the presence of bulky long cracks
dispersed across the entire particle. These cracks may be
attributed to absorption of microwave energy by the
DESs which occur more rapidly and completely.
Similar behavior was also found in extraction of baicalin
from Scutellaria baicalensis Georgi using MADESE
(Wang et al., 2018). In this process, the extraction time
was shorter than the time taken by heating and stirring
method and also higher yield was achieved with MAE.
MAE results also represent that the material cells
were effortlessly disrupted in DES conditions as DESs
break the cell wall with fiber dissolution (Gunny et al.,
2015) and the bioactive compounds were extracted from
the biomass waste. Swatloski et al. (2002) also demon-
strated that cell rupture had a significant effect on extrac-
tion and subsequently increasing the efficiency.
Figure 4(d) and (e) illustrated the void space distribu-
tion of treated sample by HSE and MADESE, respect-
ively. The void space distribution of HSE and MADESE
was determined from the SEM image of Figure 4(b) and
(c), respectively. The maximum porous area on the
sample surface was observed with size ranging from 3
to 12 mm2 in HSE while in MADESE, this porous area
might be increased up to 225 mm2. This is due to the
pressure induced by microwave radiations, leading to
the rupture of sample surface which results in release
of phenolic compounds (PCs) and thereby enhanced
yield. Maximum disruption was observed in the range
of 1–100 mm2 in MADESE.
Effect of extracts on the oxidation of
sunflower oil
An induction period of 4.02 h for sunflower oil mixed
with purified extract was reported as compared to
87
Food Science and Technology International 26(1)

(a) mV(x10)

Mangniferin/4.249
3.0

2.0

1.0

0.0
0.0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0

(b) mV(x0.1)
Mangniferin/4.245

2.0

1.0

0.0

–1.0

–2.0
0.0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0

Figure 3. (a) HPLC chromatogram of commercial standard compound and (b) HPLC chromatogram of mango peel
extracts by MADESE.

2.26 h for sunflower oil (Electronic supplementary
material Figure S3(a) and (b)).The large induction
time represents higher antioxidant activity. Taha et al.
(2010) and Sun and Ho (2005) also found a similar
trend while studying antioxidant activity of different
plant materials. Purified extract retarded the oxidation
of sunflower oil and increased the induction time.
Diagnostics of model adequacy
As shown in Electronic supplementary material Figure
S4, the diagnostic plots of TPC (a–f), FRAP (g–l), and
DPPHsc% (m–r) for the model adequacy. Raw resi-
duals depict the deviations between observed and
expected values and it cannot be explained by the
model. Figure S4 (a, g, m) represents the deviations
between experimental and predicted values. The max-
imum raw residual values obtained in this study for
TPC, FRAP, and DPPHsc% were 1.14, 14.78, and
0.14, respectively. The predicted data are very nearer
to observed data and all the points of predicted and
experimental response fall quite close to the 45 line.
The residuals following a normal distribution were
demonstrated by the normal probability plot in Figure
S4 (b, h, n). From the plot, it can be easily seen that the
there is no difference of variance as all the points lie
very close to the straight line. They represent the spe-
cific arrangement analogous to ‘‘S-shaped’’ curvature,
which indicates revolution of the reaction may give an
exceptional analysis (Maran et al., 2013). Visual assess-
ment of the diagram is sufficient and statistical tests are
not used for this diagnostic. Externally studentized resi-
duals are the best metric to use for this plot. Internally
studentized and raw residuals are available but not
recommended.
Figure S4 (c, i, o) illustrates the plot of residuals
versus experimental run order. The plot seems to be a
random scatter. The plot shows the responses being
affected by lurking variables during the experiment.
All the data points are lying in the range of 2 to 2
of the internally studentized residuals with respect to
experimental runs. This relation shows the good fit
of the model was analyzed and the entire data points
lie within the limits. Small residual value indicates
that the model prediction is accurate (Herbach et al.,
2004). Leverage values of TPC, FRAP, and DPPHsc%
are less than 1 which is represented in Figure S4
(d, j, p). Therefore, there are no unpredictable errors

88
 Pal and Jadeja

(a) (b)

5
(c)
(d)
4

Frequency
3

0
0 2 4 6 8 10 12
Void space (mm2)

10

(e)
8

6
Frequency

0
0 25 50 75 100 125 150 175 200 225
Void space (mm2)

Figure 4. SEM images of ripe mango peel samples: (a) Fresh mango peel powder, (b) residual mango peel from HSE,
(c) residual mango peel from MADESE, (d) void space distribution of HSE-based residual mango peel, and (e) void space
distribution of MADESE-based residual mango peel.

in the model. The leverage confirmed the possibility observation but that is an ideal condition (Maran et al.,
for a design point to impact the model fit and it is 2013).
lying between 0 and 1. When any model has In this study, DFBETAS diagnostic shows the influ-
achieved leverage value of 1, the model exactly fits the ence of each observation on a specific predictor.

89
Food Science and Technology International 26(1)
The regression coefficient calculated for all the data rep-
resents the variation between predictor and specific obser-
vation. It is known for ‘‘difference in betas’’; ‘‘beta’’ is one
type of coefficient. A high DFBETAS points out that the
coefficient for that term is changing because of impact
from the run. Nevertheless, diversity in beta values plot
in Figure S4 (e, k, q) explains not much impact of any
check up on any of the regression coefficients. The max-
imum Cook’s distance values for TPC, FRAP, and
DPPHsc% are observed approximately as 0.6, 2.0, and
0.4, respectively, as clearly mentioned in Figure S4 (f, l, r).
They have no effect on the responses as all the data points
are in the determined range and no clear patterns were
found in the analysis (Maran et al., 2013).
CONCLUSIONS
In this investigation, the impact of parameters like
microwave power, time, and liquid-to-solid ratio on
the three main responses TPC, FRAP, and
DPPHsc% while recovering natural antioxidant poly-
phenols from mango peels was investigated. Microwave
power is a powerful tool which efficiently improves the
extraction yield. BBD featured by three factors and
three levels was successfully employed to optimize the
extraction. The optimized conditions were as follows:
microwave power (A) of 436.45 W, irradiation time (B)
of 19.66 min, and liquid-to-solid ratio (C) of
59.82 mg l1.TPC, FRAP, and DPPHsc% values
obtained were 56.17 mg GAE g1 dw, 683.26 mmol
AAE g1 dw, and 82.54 DPPHsc%, respectively,
under these optimal conditions. These data are very
close to the experimental values obtained under the
optimized conditions. The oxidative stability of sun-
flower oil was increased from 2.26 to 4.02 h by the add-
ition of purified extracts of mango peel. These results
showed that mango peels could be used as a potential
dietary source of antioxidants.
ACKNOWLEDGEMENT
The authors gratefully acknowledge the support of Dr N. A.
Gajbhiye, Senior Scientist (Organic Chemistry), ICAR-
Directorate of Medicinal & Aromatic Plants Research,
Anand, Gujarat by providing necessary facilities for HPLC
analysis of the samples and help rendered in analytical
determinations.
DECLARATION OF CONFLICTING INTERESTS
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of this
article.
FUNDING
The author(s) received no financial support for the research,
authorship, and/or publication of this article.
90
ORCID ID
Girirajsinh C Jadeja https://orcid.org/0000-0002-1973-
8166
SUPPLEMENTAL MATERIAL
Supplemental material for this article is available online.
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