Food Research International 119 (2019) 455–461

Contents lists available at ScienceDirect

Food Research International

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

Sequential extraction of phenolics and pectin from mango peel assisted by T

ultrasound
⁎
Bruna Bárbara Valero Guandalini, Naira Poerner Rodrigues , Ligia Damasceno Ferreira Marczak
Chemical Engineering Department, Federal University of Rio Grande do Sul (UFRGS), Ramiro Barcelos Street 2777, 90036-007 Porto Alegre, Rio Grande do Sul, Brazil

A R T I C LE I N FO A B S T R A C T

Keywords: The present work evaluated the use of ultrasound to extract sequentially phenolics and pectin from mango peel.
Mangifera indica L. Initially, the influence of ethanol and ultrasound on the phenolics extraction was investigated. The results
Processing waste showed that the ultrasound did not affect the extraction yield of these compounds. The best total phenolics yield
Antioxidant (67%) was obtained with an extraction solution consisting of 50% of ethanol in water (v/v) and without ul-
Dietary fiber
trasound application, according to the experimental design. As an innovative extraction methodology, the re-
Emerging technologies
Galacturonic acid
sidue of this extraction was then used to extract pectin assisted by ultrasound. The use of ultrasound increased
over than 50% of the pectin extraction yield and did not affect its quality, measured by the galacturonic acid
content and the degree of esterification. The sequential extraction of phenolics and pectin shows to be an al-
ternative to use the whole residue from mango peel.

1. Introduction microbial and antioxidant activity. Moreover, the phenolic compound

Mango (Mangifera indica L.) is one of the most important tropical
fruits with 51 millions of tons produced in the world in 2016, according
to Food and Agriculture Organization (FAO, 2016). Brazil is the second
largest producer in America and the seventh in the world. Due to its
high perishability and seasonality, mango pulp is widely processed in
products such as nectar, juice, puree and mango desserts. The waste
generated by the mango pulp processing includes peel, kernel and ba-
gasse, which comprises 35–60% of the total fruit weight, producing a
large disposal problem (Larrauri, Rupérez, Borroto, & Saura-Calixto,
1996). Mango peel represents 15 to 20% of the fruit weight and there is
no commercial application for this waste (Pandit, Vijayanand, &
Kulkarni, 2015).
Mango peel is reported to have good amount of bioactive com-
pounds, which makes it suitable to be processed for value-added ap-
plications in functional foods and nutraceuticals (Berardini, Knödler,
Schieber, & Carle, 2005; Sogi, Siddiq, & Dolan, 2015). It is rich in
carotenoids and phenolic compounds with excellent antioxidant and
functional properties (Ajila, Aalami, Leelavathi, & Rao, 2010;
Mahattanatawee et al., 2006; Pardo Andreu, Delgado, Velho, Curti, &
Vercesi, 2005). Phenolic compounds are produced through the sec-
ondary metabolism of plants and are essential for their growth. This
group of biologically active molecules has been extensively studied due
to their multiple biological effects, such as anti-inflammatory, anti-
can be used by the food industry as a substitute for synthetic anti-
oxidants (Rafiee, Barzegar, Ali, & Maherani, 2017).
Pectin is another important compound presented in mango peel,
which is a polysaccharide widely used in food industry as a gelling,
stabilizing and thickening agent. Pectin is a natural anionic hydro-
colloid existing in primary cell walls of dicotyledonous plants. This
soluble fiber consists of a backbone of α (1 → 4) galacturonic acid
which are partially esterified with methyl alcohol or acetic acid in
carboxyl group (Khorasani & Shojaosadati, 2017; Thakur, Singh,
Handa, & Rao, 1997; Zdunek, Kozioł, Pieczywek, & Cybulska, 2014).
According to FAO, commercial pectin must contain at least 65% of
galacturonic acid (JECFA, 2016). Another pectin classification refers to
the degree of esterification (DE), which represents the carboxyl groups
of the main chain of galacturonic acid that are esterified with methyl or
acetyl groups (Farris, Schaich, Liu, Piergiovanni, & Yam, 2009). Pectin
can be classified as high methoxyl pectin (DE > 50%) or low methoxyl
pectin (DE < 50%); the DE affects gelling properties of pectins. The
food industry uses mainly the pectin with high methoxyl content
(Videcoq, Garnier, Robert, & Bonnin, 2011). In addition to its techno-
logical properties, pectin is suggested to have various pharmaceutical
properties, including wound healing, lipase inhibition and cholesterol
decreasing effects (Isaksson, Lundquist, Akesson, & Ihse, 1982; Keys,
Grande, & Anderson, 1961).
The conventional techniques for extracting bioactive compounds

⁎
Corresponding author.
E-mail address: nairapoernersa@gmail.com (N.P. Rodrigues).

https://doi.org/10.1016/j.foodres.2018.12.011
Received 30 May 2018; Received in revised form 22 November 2018; Accepted 9 December 2018
Available online 11 December 2018
0963-9969/ © 2018 Elsevier Ltd. All rights reserved.
B.B.V. Guandalini et al.
include direct boiling, solvent maceration, distillation, compression,
among others (Chemat et al., 2017). These processes are time con-
suming and can cause degradation of thermolabile compounds. Ultra-
sound-assisted extraction is a process that uses acoustic energy and
solvents to enhance the release and diffusion of target compounds from
various matrices. The enhancement of the mass transfer is brought
about by the acoustic cavitation induced in a liquid medium (Laborde,
Bouyer, Caltagirone, & Gérard, 1998; Lopez-Avila, Young, & Teplitsky,
1995).
The extraction of bioactive compounds from mango peel of different
varieties has been studied by many authors. Some examples include the
extraction of phenolic compounds (Ajila, Naidu, Bhat, & Rao, 2007;
Aziah, Aziz, Wong, Bhat, & Cheng, 2012; Garcia-Mendoza, Paula,
Paviani, Cabral, & Martinez-Correa, 2015; Sogi et al., 2015), car-
otenoids (Ajila et al., 2007; Aziah et al., 2012; Garcia-Mendoza et al.,
2015; Sogi et al., 2015) and pectin (Pandit et al., 2015). To the best of
our knowledge there are no studies carried out to investigate the se-
quential extraction of these bioactive compounds. The sequential ex-
traction is an alternative for better use of mango peel, since it is possible
to obtain an extract rich in phenolics and reuse this residue for the
pectin extraction. In this way, it is possible to obtain two bioactive
compounds from the mango peel.
In this context, the aim of this study was to evaluate the effect of the
ultrasound as an alternative technology on the sequential extraction of
phenolics and pectin from mango peel of Tommy Atkins cultivar.
Initially, the phenolics were extracted from mango peel using the ul-
trasound power intensity and the ethanol volume fraction as in-
dependent variables within the experimental design. After, the pectin
was sequentially extracted from the residue obtained in the phenolics
extraction. The influence of the previous phenolics extraction and the
use of ultrasound on the yield and quality of mango pectin were eval-
uated to verify the effectiveness of the sequential extraction.
2. Material and methods
2.1. Plant material
Tommy Atkins mangoes were harvested in Juazeiro city, Bahia state
(latitude 09°24′50” S, longitude 40°30′10” W, 368 m altitude). The
fruits were purchased from a local market (Porto Alegre, RS, Brazil).
The fruits were washed, sanitized in sodium hypochlorite solution
(200 ppm) for 20 min and peeled with a stainless-steel knife. The pulp
excess was removed from the peel with a spoon; the peel was chopped
into square pieces of approximately 1 cm2 and packed in polypropylene
bags. The bleaching of the peels was performed by immersion in water
bath at 85 °C for 3 min followed by cooling in an ice bath. The peels
were drying in a convective oven with air circulation (Solab cientifica,
sl 102/100, Brazil) at 60 °C up to constant weight (~40 h). The dried
mango peels were then milled and sieved (< 4 mm) and packaged in
polypropylene bags, protected from light, and storage a −18 °C, until
use. Part of the dried mango peel was milled again and sieved
(< 0.25 mm) to perform the phenolics exhaustive extraction. The final
moisture content of the mango peel was 4.3 ± 0.2 g/100 g.
2.2. Phenolics extraction
2.2.1. Exhaustive extraction of phenolics
In order to obtain the total phenolic content of mango peel, the
exhaustive extraction was performed using the methodology describe
by Rodrigues, Mariutti, and Mercadante (2013). Milled (< 0.25 mm)
dried mango peel (0.1 g) was extracted with 10 mL of methanol/water
mixture (8:2, v/v) by agitation for 5 min followed by centrifugation at
10,000g for 10 min. The solid residue was re-extracted with a fresh
solvent and each supernatant was evaluated by Folin-Ciocalteu method,
until no absorbance was detected. The exhaustive extraction was ob-
tained after 5 re-extractions and the quantification of total phenolics
456
Food Research International 119 (2019) 455–461
was determined spectrophotometrically according to the Folin-Cio-
calteu method (described in Section 2.2.3).
2.2.2. Ultrasound-assisted extraction of phenolics
The application of ultrasound was performed using an ultrasound
probe with 13 mm of diameter and constant frequency of 20 kHz
(Sonics & Materials Inc., VC750, USA). The ultrasound extraction was
performed in an extraction cell made of Pyrex glass, with a water jacket,
placed on a magnetic stirrer (IKA®, C-MAG HS10, Germany) to avoid
overheating zones. The extraction cell was connected to two thermo-
static baths, one at 5 °C and other at 30 °C, in order to maintain the
temperature constant throughout the extraction experiment.
Ultrasound-assisted extraction of phenolics from mango peel was
performed using the following conditions: dried peel/solvent ratio 1:25
(g/mL) and temperature of 30 °C. Previously to extraction, the dried
mango peel (4 g) was rehydrated with 25 mL of water during 20 min in
the extraction cell. Then, 75 mL of an ethanol/water mixture was added
in order to obtain an extraction solution consisting of 25–75% of
ethanol volume fraction in water (v/v). The magnetic stirrer was
switched on and the ultrasound applied for 20 min. The extraction of
total phenolic was monitored by collecting extracts (1 mL) after 2, 5, 8,
10, 15 and 20 min. Each extract was immediately centrifuged
(Eppendorf AG, MiniSpin®, Germany) at 12,000g for 3 min at room
temperature (T < 25 °C) and the supernatant was used in the analysis
of total phenolic content by the Folin-Ciocalteu method.
A 32 factorial experimental design was conducted in order to opti-
mize the extraction of total phenolics. The studied variables were the
ultrasound power intensities (165.87 W/cm2, 331.6 W/cm2 and
497.4 W/cm2, corresponding, respectively, to 25%, 50% and 75% of the
maximum power of the equipment) and the ethanol volume fraction
(25%, 50% and 75% (v/v)) in the aqueous extraction solution. All the
experiments were carried out in duplicate, randomly. The analyses of
each independent sample were performed in triplicate. The results were
analyzed using the software Statistica ® (13.0, Statsoft Inc., USA) and
experimental data were fitted to the polynomial regression model
showed in Eq. 1:
Y = β0 + β1 X1 + β2 X2 + β11 X12 + β22 X22 + β12 X1 X2 (1)
where Y represents the total phenolic content, X1 is the real variable for
ultrasound power intensity, X2 is the real variable for ethanol volume
fraction, and β0, β1, β2, β11, β22 and β12 represent the equation coeffi-
cients.
The statistical significance of the terms in the regression equation
was determined by ANOVA with a 95% of confidence level. The terms
statistically found as non-significant were excluded from the initial
model and the experimental data were re-fitted using only the sig-
nificant (p < 0.05) parameters.
2.2.3. Determination of the total phenolic content
The total phenolic content was determined using the colorimetric
method of Folin-Ciocalteu (Singleton & Rossi, 1965). The reaction
mixture was prepared by mixing the extract, the Folin-Ciocalteu re-
agent 2 N (5%, v/v) and the Na2CO3 solution (3%, m/v). The reaction
mixture was kept in the dark at room temperature (T < 25 °C) for 1 h
and the absorbance signal was read at 765 nm using a UV-VIS spec-
trophotometer (PG Instruments Ltd., T80 UV–Vis, United Kingdom).
The quantification was carried out using an analytical curve for gallic
acid in the range of 1–9 μg/mL, and the total phenolic content was
expressed in milligrams of gallic acid equivalent (GAE) per gram of
mango peel on dry base (d.b.).
The best condition of the phenolic compounds extraction (50% of
ethanol in water and no application of ultrasonic waves) was used to
perform the sequential extraction of pectin (which is the main objective
of the present work). This sequential extraction was accomplished using
the residue of the phenolics extraction and the ultrasound effect in the
B.B.V. Guandalini et al.
pectin extraction was investigated. The yield and the quality of the
pectin sequentially extracted were compared with the results obtained
in the direct extraction from the dried mango peel (without a prior
phenolics extraction). In the following it will be presented the meth-
odologies for the pectin extraction.
2.3. Pectin extraction
Ultrasound-assisted pectin extraction was performed in the mango
peel and in the residue of the phenolics extraction using the metho-
dology proposed by Freitas de Oliveira et al. (2016) with some mod-
ifications. 3.3 g of the mango peel (previously rehydrated with 25 mL of
water during 20 min) or 3.3 g of the phenolics extraction residue were
put into the extraction cell with nitric acid solution (1.0 M, pH 2.00) to
complete 100 mL. The extraction cell was connected with two water
baths in order to maintain the temperature at 85 ± 2 °C throughout the
extraction experiment. The extraction was performed using 75% of
ultrasound intensity (497.4 W/cm2) during 10 min with constant stir-
ring.
In order to evaluate the ultrasound effect in pectin extraction,
control experiments were performed using the same experimental
conditions without the application of ultrasound. The conventional
pectin extraction was performed using the mango peel under identical
conditions, but for 30 min.
After ultrasound, control and conventional extraction, the samples
were cooled to 10–15 °C, centrifuged and filtrated. The extracted pectin
was precipitated by adding two volumes of ethanol (95%) to the su-
pernatant; the mixture with the precipitated pectin was stored in a
refrigerator at 4 °C for 30 min, separated by vacuum filtration and im-
mersed in an ethanol solution (70%) for 12 h to remove the impurities.
The purified pectin was dried in an oven with air circulation at 40 °C up
to constant weight.
The extraction yields were calculated according to the following
equation:
Yield (%) = pectin weigtht (g )/ sample weight (g ) × 100 (2)
2.4. Pectin characterization
For analyzes of galacturonic acid content, degree of esterification
and color the dried pectin (50 mg) was solubilized in 100 mL of distilled
water at 50 °C with constant stirring, until it was completely dissolved
(~30 min).
2.4.1. Determination of galacturonic acid
Galacturonic acid (GalA) was determined according to m-hydro-
xydiphenyl method (Blumenkrantz & Asboe-Hansen, 1973). Samples of
pectin (500 μL) were thoroughly mixed with 3.0 mL of 0.125 M sodium
tetraborate solution (in concentrated sulfuric acid), heated for 5 min
and immediately cooled in an ice bath. Then, 20 μL of 0.15 g/100 mL m-
hydroxydiphenyl (in 0.5 g/100 mL NaOH) was added to the pectin so-
lution and, after 5 min, the absorbance signal was read at 520 nm using
an UV spectrophotometer (PG Instruments Ltd., T80 UV–Vis, United
Kingdom). Quantification was carried out using an analytical curve for
galacturonic acid in the range from 2 to 100 μg/mL.
2.4.2. Degree of esterification
The degree of esterification (DE) was determined using the titri-
metric method (Bochek, Zabivalova, & Petropavlovskii, 2000). The di-
luted pectin (100 mL) was titrated with 0.05 M sodium hydroxide to
pH 8.5 ± 0.2 (monitored using a digital pHmeter, Digimed, Model
DM22) and this volume was recorded as initial titer (V1). Then, 10 mL
of 0.5 M sodium hydroxide was added to the solution that was shaken
vigorously, allowed to stand for 15 min at 30 °C, and neutralized with
10 mL of 0.5 M hydrochloric acid. Phenolphthalein was added and the
solution was titrated with 0.5 M sodium hydroxide to a faint pink color.
457
Food Research International 119 (2019) 455–461
This volume was recorded as final volume (V2). The DE was calculated
using Eq. 3:
V2
DE (%) = × 100
V1 + V2 (3)
2.4.3. Color analyses
The pectin color measurement was performed using a ColorQuest
XE colorimeter (Hunter Assoc. Laboratory, VA, USA). The CIELAB
colorimetric parameters L*, a* e b* were obtained, using the trans-
mittance mode, with the light source D65 and observation angle of 10°.
The parameters chroma (Cab∗), hue angle (hab) and total color differ-
ence (ΔE) were calculated using the following equations.
∗
Cab = (a∗)2 + (b∗)2 (4)
hab = tan−1 (a∗/ b∗) (5)
∆E = (∆a∗)2 + (∆b∗)2 + (∆L∗)2 (6)
2.5. Statistical analysis
All the experiments were performed at least in duplicate, and the
analyses of each independent sample were performed in triplicate. The
results were submitted to the analysis of variance (ANOVA) and the
means were compared by Tukey's test with a 95% of confidence level
using the software Statistica ® (13.0, Statsoft Inc., USA).
3. Results and discussion
3.1. Total phenolics extraction
The effects of ultrasound intensity and ethanol volume fraction on
the phenolics extraction from mango peel were investigated by a fac-
torial experimental design 32. The total phenolic content was de-
termined after 2, 5, 8, 10, 15 and 20 min of extraction and the results
are presented in Fig. 1. The statistical analysis of the data, considering a
significance level of 5%, showed that the total phenolics amount ex-
tracted increased in the first 8 min for almost all treatments studied. For
longer periods of time (10, 15 and 20 min), the content extracted did
not increase significantly. Thus, the total phenolics extraction condi-
tions were optimized using the responses at 8 min of extraction.
The results of the factorial experimental design are shown in
Table 1. Each extraction condition of the experimental design was
performed in duplicate and the coefficient of variation was lower than
10%, indicating good repeatability of the extraction process. The total
phenolic content extracted from mango peel ranged from 6.0 (run 8) to
9.8 (run 4) mg GAE/g d.b., corresponding, respectively, to 44% and
73% of the total phenolics present in mango peel (exhaustive extrac-
tion).
The total phenolic content was fitted to a second-order model (Eq.
1) and evaluated in terms of the fit goodness. Table 2 presents the re-
gression coefficients for the effects of ultrasound power intensity and
ethanol volume fraction on total phenolics extraction. As can be seen,
the linear and the quadratic terms for ethanol volume fraction were
significant, while the power intensity of ultrasound had no significant
effects (considering a significant level of 5%).
The model adequacy was checked by F-test and by the determina-
tion coefficient R-squared. The results for ANOVA led to value
F = 53.68 greater than F tabulated (Ft = 6.94), which demonstrated
significance for the regression model and that the model, given by Eq.
7, is predictive. The R-squared value was 0.865; according to Myers,
Montgomery, and Anderson-Cook (2002) a value of R-squared > 0.750
indicates the aptness of the model. Also, the lack of fit did not present
significance (p < 0.05).
B.B.V. Guandalini et al. Food Research International 119 (2019) 455–461

14

12

Total phenolic content (mg GAE/g d.b.)

10

0
0 2 4 6 8 10 12 14 16 18 20
Time (min)

Fig. 1. Kinectics of the total phenolic content extracted from mango peel at different ultrasound intensities and ethanol volume fractions. Legend: 50% ethanol – 50%
power (filled lozenge), 25% ethanol – 50% power (filled square), 75% ethanol – 50% power (open triangle), 50% ethanol – 75% power (filled triangle), 25% ethanol
– 75% power (filled circle), 75% ethanol – 75% power (open lozenge), 50% ethanol – 25% power (open circle), 75% ethanol – 25% power (open square), 25%
ethanol – 25% power (cross).

Table 1 is presented in Fig. 2. As can be observed, the range from 50% to 60% of
Total phenolic content on the extracts and the extraction yield after application ethanol volume fraction was the best for the phenolics extraction, and
of different ultrasound intensities and ethanol volume fractions, at 8 min of the ultrasound power intensity did not significantly (p > 0.05) affect
extraction. the total phenolic content extracted.
Run Ethanol Ultrasound Total phenolic content Yield Thus, considering that the ultrasound power intensity did not affect
volume intensity (%) (mg GAE/g, d.b.)⁎ (%)⁎⁎ the phenolics extraction, and aiming to reduce the solvent and energy
fraction (%) expenditure, the best condition to the phenolics extraction from mango
peel was chosen to be 50% of ethanol volume fraction and no appli-
1 75 75 8.60 ± 0.06abc 62
2 75 50 8.4 ± 0.8abc 61 cation of ultrasonic waves. In order to verify the predictive capacity of
3 75 25 7.4 ± 0.3bcde 52 the model, experiments were performed (in triplicate) using these
4 50 75 9.8 ± 0.4a 73 conditions and 9.3 ± 0.4 mg GAE/g d.b. of the total phenolics was
5 50 50 9.6 ± 0.4ab 69
extracted; the model provided a value of 8.7 mg GAE/g d.b. The dif-
6 50 25 9.3 ± 0.8ab 71
7 25 75 6.2 ± 0.8de 41
ference between the experimental and predicted values is lower than
8 25 50 6.0 ± 0.8e 44 6.5%, confirming the predictability of the model obtained. It is worth
9 25 25 6.44 ± 0.03cde 47 point out that the value obtained in the optimized condition corre-
Exhaustive extraction 13.82 ± 0.08 – sponds to 67% of the total amount of phenolics present in mango peel
⁎ (exhaustive extraction).
Mean ± standard deviation; means with the same lowercase letter in the
Espada-Bellido et al. (2017) optimized the extraction process of
same column do not have significant difference (p > 0.05).
⁎⁎
Extraction yield of total phenolics, comparison with the exhaustive ex- anthocyanins and total phenolic compounds present in mulberries.
traction. Several extraction variables were evaluated including extraction solu-
tion composition, temperature and ultrasound amplitude. Extraction
Table 2 temperature and solvent composition were found to be the most in-
Regression coefficient for phenolics extracted from mango peel. fluential parameters for extraction of these compounds. In accordance
with the results obtained in the present work, the ultrasound power did
Factor Regression Standard t-value p-value
coefficient error
not affect significantly the total phenolics extraction.
(p < 0.05) The extraction of phenolic compounds in artichoke waste was
evaluated by Rabelo, Machado, Martínez, and Hubinger (2016). The
Mean 7.93 0.12 65.95 0.0000 research aimed to study the potential of sequential process based on the
Ultrasound intensity (L) 0.24 0.30 1.62 0.129
Ultrasound intensity (Q) −0.02 0.25 −0.20 0.847
use of ultrasound extraction and membrane technology. The results
Ethanol volume fraction 0.95 0.30 6.32 < 0.05 showed that the ultrasound power higher than 240 W had no influence
(L) on the process efficiency and that the most important parameter was
Ethanol volume fraction 1.15 0.25 9.25 < 0.05 the solvent composition (ethanol/water ratio), as observed in the pre-
(Q)
sent work.
Ultrasound intensity x 0.37 0.37 1.99 0.067
Ethanol volume
fraction (L) 3.2. Extraction and characterization of mango peel pectin
L: linear term. Q: quadratic term.
Table 3 presents the pectin yield, the galacturonic acid content
Phenolic compound = 7.94 + 0.95∙Et + 1.15∙Et 2 (GalA) and the degree of esterification (DE) of the pectin extracted from
(7)
the rehydrated mango peel (RMP) and from the residue obtained from
The response surface for total phenolics extraction from mango peel the previous phenolics extraction (PER, phenolics extraction residue).

458
B.B.V. Guandalini et al.
Fig. 2. Response surface (a) and contour diagrams (b) for total phenolics extracted from mango peel as a function of ultrasound intensities and ethanol volume
fractions, at 8 min of extraction.
The pectin extractions were performed using ultrasound with intensity
of 75% and without the application of ultrasound (control). As can be
observed, the pectin yield extracted from the PER and from the RMP,
within the same extraction method (ultrasound or control), is not sig-
nificantly different. This indicates that the previous phenolics extrac-
tion performed at 30 °C in aqueous ethanol did not remove the pectin
from the vegetable matrix. Regarding the pectin quality parameters, it
can be seen that, for the same extraction method, there is no difference
in the GalA content and in the DE of the pectin extracted from PER and
RMP. These results indicated that pectin quality was not affected by the
previous extraction of phenolics from mango peel.
Concerning the comparison between the extraction performed with
and without ultrasound, it can be seen that the use of this technology
enhanced in 53% (from 5.6% to 8.6%) and in 31% (from 6.2% to 8.1%)
the pectin yield extracted from the PER and RMP, respectively.
According to many studies, the ultrasound technique improves the ex-
traction of target compounds from plant tissues (Jaeschke, Rech,
Marczak, & Mercali, 2017; Lazar, Talmaciu, Volf, & Popa, 2016;
Moorthy et al., 2017; Wang et al., 2016). The enhancement of the mass
transfer is brought about by the acoustic cavitation, produced by the
expansion-compression cycles, in a liquid medium. The collapse of the
bubbles induces a faster liberation of recoverable compounds. More-
over, the probably synergy between ultrasound and heating may in-
crease the solubility of numerous compounds, improving the mass
transfer.
It can also be seen in Table 3 that the GalA content present in the
PER and RMP ranged from 63% to 76%. According to FAO (JECFA,
2016), the polymer must have at least 65% of GalA content to be
classified as commercial pectin. Considering the standard deviation
Table 3
Characterization of mango peel pectin obtained by conventional extraction, ultrasound assisted and control extraction.
Analyses⁎ Ultrasound 75%
Phenolics extraction residue Rehydrated mango peel
(PER) (RMP)
Pectin yield (%) 8.6 ± 0.3a 8.1 ± 0.6a
GalA (%) 70 ± 3ab 76 ± 5ab
DE (%) 58 ± 4 a 61 ± 6 a
⁎
The results represent the average of triplicates ± standard deviation. Results followed by different small letters in the same line indicate significant difference
(p < 0.05) according to Tukey's test.
Food Research International 119 (2019) 455–461
associated with the minimum value, all polymers extracted from mango
peel in the present work can be categorized as commercial pectin.
Moreover, the GalA content was not influenced by the ultrasound ap-
plication, which is a good result considering the objective of the present
work.
To the best of our knowledge, there is no works in the literature
which extracted pectin from mango peel of the Tommy Atkins variety
with GalA content > 65%. In fact, many studies have already pointed
out the difficulty in adjusting the process parameters to achieve the
minimum GalA content of 65% in the mango peel pectin (Jamsazzadeh
Kermani, Shpigelman, Pham, Van Loey, & Hendrickx, 2015; Nagel
et al., 2014; Wang et al., 2016). Geerkens et al. (2015) evaluated the
influence of the cultivar, ripeness, peel particle size, blanching, drying
and irradiation on pectin quality of the Tommy Atkins mango peel. The
authors found that the reduction of peel particle size, the blanching and
the ripening increased the GalA content, but the maximum content
obtained was 48%. In other mango varieties, as Maha Chanok and Nam
Dokmai, Geerkens et al. (2015) evaluated 19 prototype processes to
pectin recovery and reported that the GalA content varied from 65% to
83%.
It is important to emphasize that, depending on the source, and,
mainly, on the experimental conditions applied during the extraction
process, the pectin will have different characteristics. The GalA content
and the degree of esterification of pectic polysaccharides affect the
commercial uses of pectin as gelling and thickening agents (Endress &
Mattes, 2009; Koubala et al., 2008; Willats, Knox, & Mikkelsen, 2006).
Regarding the degree of esterification (DE), it was observed that, for
all pectin extracted, the DE varied between 58% and 67%, indicating
that they are classified as high methoxyl pectin. This pectin forms gel
Control Conventional extraction
Phenolics extraction residue Rehydrated mango peel Rehydrated mango peel (RMP)
(PER) (RMP)
5.61 ± 0.07b 6.2 ± 0.5b 5.4 ± 0.4b
66 ± 3b 63 ± 5b 80.71 ± 0.09a
64 ± 3a 67 ± 4a 67 ± 1a
459
B.B.V. Guandalini et al.
Table 4
Color parameters of pectin extracted from mango peel assisted by ultrasound, control and conventional method.
Parameters⁎ Ultrasound 75%
Phenolics extraction residue Rehydrated mango peel
(PER) (RMP)
L⁎ 94.36 ± 0.04b 94.5 ± 0.1b
a⁎ −0.29 ± 0.06a −0.36 ± 0.07a
b⁎ 4.3 ± 0.3a 4.9 ± 0.8a
Cab⁎ 4.3 ± 0.3a 4.9 ± 0.8a
hab 95 ± 1a 94.2 ± 0.1a
⁎
The results represent the average of triplicates ± standard deviation. Results followed by different small letters in the same line indicate significant difference
(p < 0.05) according to Tukey's test.
with high amount of sugar (65% or more) and low pH and it is normally
used for jellies, jams and products with high sugar concentration.
In Table 3 it is also presented the pectin yield and quality para-
meters obtained by a conventional extraction using the rehydrated
mango peel and a comparison with the experiment using ultrasound
75% can be accomplished. As can be observed, the use of ultrasound
increased the yield in 50% (from 5.4% to 8.1%) and did not influence
the quality parameters. It is important to point out that the conven-
tional extraction lasts 30 min while the ultrasound assisted extraction
lasts only 10 min. These results demonstrated that the ultrasound was
an efficient and time saving technique for extraction of pectin from
mango peel.
A similar analysis, considering the extraction with and without the
application of ultrasound, from the PER and the RMP, and a conven-
tional extraction, was performed to investigate changes in the pectin
color parameters. These results are presented in Table 4. The hue angle
(hab) varied from 93.8 to 96, showing that the color of the pectins was
yellowish, regardless of the extraction treatment applied. Moreover,
none of the color parameters analyzed for the mango peel pectin were
significantly affected by the previous phenolics extraction, considering
the same extraction method.
The pectin extracted by ultrasound from PER and RMP presented
darker coloration (lower luminosity, L*), are yellower (higher b*) and
presented higher saturation (higher chroma Cab∗) when compared with
the conventional and the control extractions. During the mango peel
drying (performed in an oven with air circulation at 60 °C) it was ob-
served visually the browning of the samples, probably due to the for-
mation of brown pigments (melanoidins) as a result of the Maillard
reaction and caramelization. The cavitation induced during sonication
may have extracted these brown pigments, conferring a darker col-
oration on the pectin extracted using ultrasound.
The pectin color change can also be confirmed by the total color
difference (ΔE) analysis which evaluated the relationship between the
visual and the numerical analysis of the L*, a* and b* parameters. The
pectin extracted by ultrasound presented ΔE values of 2.8 (PER) and 3.3
(RMP) when compared with the conventional extraction and ΔE values
of 2.8 (PER) and 3.1 (RMP) when compared with the control extraction.
According to the standard DIN 6174 (DIN, 1979) values of ΔE between
1.5 and 3.0 represent a perceptible visual color change. Therefore, the
pectin extracted by ultrasound presented a perceptible color change
when compared with the pectin extracted by conventional and control
extractions.
4. Conclusions
Ultrasound extraction, as an emerging technology, was applied to
extract sequentially phenolics and pectin from mango peel. The ultra-
sound did not affect the extraction of the total phenolics, with the best
yield (67%) being obtained with 50% of ethanol volume fraction in
water without ultrasound application. Concerning the pectin extracted
with and without ultrasound, the use of this technology enhanced in
Food Research International 119 (2019) 455–461
Control Conventional extraction
Phenolics extraction residue Rehydrated mango peel (RMP) Rehydrated mango peel (RMP)
(PER)
95.7 ± 0.1a 95.69 ± 0.05a 95.76 ± 0.04a
−0.18 ± 0.06a −0.193 ± 0.004a −0.19 ± 0.01a
1.9 ± 0.2b 2.06 ± 0.06b 1.9 ± 0.3b
1.9 ± 0.2b 2.06 ± 0.06b 1.9 ± 0.3b
93.8 ± 0.5a 95.37 ± 0.07a 96 ± 1a
53% (from 5.6% to 8.6%) and in 31% (from 6.2% to 8.1%) the pectin
yield extracted from the phenolics extraction residue and from the re-
hydrated mango peel, respectively. Regarding the pectin quality para-
meters, the ultrasound did not affected the GalA content and DE, but
the pectin presented a perceptible color change. It was observed that
the previous phenolics extraction did not affect the yield and pectin
quality parameters (GalA, DE and color parameters). Regardless of the
extraction method applied, all pectin extracted from Tommy Atkins
mango peel can be categorized as commercial pectin (GalA > 65%).
These results demonstrated that the sequential extraction of phenolics
and pectin could be an alternative to use the whole mango peel from
the industry to obtain an extract rich in phenolics and a commercial
pectin.
Acknowledgments
The authors gratefully acknowledge the financial support received
from CAPES (Coordenação de Aperfeiçoamento de Pessoal de Nível
Superior, Brazil), CNPq (Conselho Nacional de Desenvolvimento
Científico e Tecnológico, Brazil) and FAPERGS (Fundação de Apoio à
Pesquisa do Rio Grande do Sul, Brazil).
References
Ajila, C. M., Aalami, M., Leelavathi, K., & Rao, U. J. S. P. (2010). Mango peel powder: A
potential source of antioxidant and dietary fiber in macaroni preparations. Innovative
Food Science and Emerging Technologies, 11(1), 219–224. https://doi.org/10.1016/j.
ifset.2009.10.004.
Ajila, C. M., Naidu, K. A., Bhat, S. G., & Rao, U. J. S. P. (2007). Bioactive compounds and
antioxidant potential of mango peel extract. Food Chemistry, 105(3), 982–988.
https://doi.org/10.1016/j.foodchem.2007.04.052.
Aziah, N., Aziz, A., Wong, L. M., Bhat, R., & Cheng, L. H. (2012). Evaluation of processed
green and ripe mango peel and pulp flours (Mangifera indica var. Chokanan) in terms
of chemical composition, antioxidant compounds and functional properties. Food
Agriculture, 557–563. https://doi.org/10.1002/jsfa.4606.
Berardini, N., Knödler, M., Schieber, A., & Carle, R. (2005). Utilization of mango peels as
a source of pectin and polyphenolics. Innovative Food Science & Emerging Technologies,
6(4), 442–452. https://doi.org/10.1016/j.ifset.2005.06.004.
Blumenkrantz, N., & Asboe-Hansen, G. (1973). New method for quantitative determina-
tion of uronic acids. Analytical Biochemistry, 54(2), 484–489. https://doi.org/10.
1016/0003-2697(73)90377-1.
Bochek, A. M., Zabivalova, N. M., & Petropavlovskii, G. A. (2000). Determination of the
esterification degree of polygalacturonic. Russian Journal of Applied Chemistry, 74,
796–799.
Chemat, F., Rombaut, N., Sicaire, A.-G., Meullemiestre, A., Fabiano-Tixier, A.-S., & Abert-
Vian, M. (2017). Ultrasound assisted extraction of food and natural products.
Mechanisms, techniques, combinations, protocols and applications. A review.
Ultrasonics Sonochemistry, 34, 540–560. https://doi.org/10.1016/j.ultsonch.2016.06.
035.
Endress, H. U., & Mattes, F. (2009). Pectin. Fiber ingredients: Food applications and health-
benefits (pp. 135–160). .
Espada-Bellido, E., Ferreiro-González, M., Carrera, C., Palma, M., Barroso, C. G., &
Barbero, G. F. (2017). Optimization of the ultrasound-assisted extraction of antho-
cyanins and total phenolic compounds in mulberry (Morus nigra) pulp. Food
Chemistry, 219, 23–32. https://doi.org/10.1016/j.foodchem.2016.09.122.
FAO (2016). Food and Agriculture Organization of the United Nations. Production quantity
of mangoes, mangosteens, and guavas. Retrieved from http://www.fao.org/faostat/
en/#data/QC.
Farris, S., Schaich, K. M., Liu, L., Piergiovanni, L., & Yam, K. L. (2009). Development of
polyion-complex hydrogels as an alternative approach for the production of bio-
460
B.B.V. Guandalini et al.
based polymers for food packaging applications: A review. Trends in Food Science &
Technology, 20(8), 316–332. https://doi.org/10.1016/j.tifs.2009.04.003.
Freitas de Oliveira, C., Giordani, D., Lutckemier, R., Gurak, P. D., Cladera-Olivera, F., &
Ferreira Marczak, L. D. (2016). Extraction of pectin from passion fruit peel assisted by
ultrasound. LWT – Food Science and Technology, 71, 110–115. https://doi.org/10.
1016/j.lwt.2016.03.027.
Garcia-Mendoza, M. P., Paula, J. T., Paviani, L. C., Cabral, F. A., & Martinez-Correa, H. A.
(2015). Extracts from mango peel by-product obtained by supercritical CO2 and
pressurized solvent processes. LWT – Food Science and Technology, 62(1), 131–137.
https://doi.org/10.1016/j.lwt.2015.01.026.
Geerkens, C. H., Nagel, A., Just, K. M., Miller-Rostek, P., Kammerer, D. R., Schweiggert, R.
M., & Carle, R. (2015). Mango pectin quality as influenced by cultivar, ripeness, peel
particle size, blanching, drying, and irradiation. Food Hydrocolloids, 51, 241–251.
https://doi.org/10.1016/j.foodhyd.2015.05.022.
Isaksson, G., Lundquist, I., Akesson, B., & Ihse, I. (1982). Influence of dietary fiber on
intestinal activities of pancreatic enzyme and on fat absorption in man. Digestion,
(39), 25.
Jaeschke, D. P., Rech, R., Marczak, L. D. F., & Mercali, G. D. (2017). Ultrasound as an
alternative technology to extract carotenoids and lipids from Heterochlorella luteo-
viridis. Bioresource Technology, 224. https://doi.org/10.1016/j.biortech.2016.11.107.
Jamsazzadeh Kermani, Z., Shpigelman, A., Pham, H. T. T., Van Loey, A. M., & Hendrickx,
M. E. (2015). Functional properties of citric acid extracted mango peel pectin as
related to its chemical structure. Food Hydrocolloids, 44, 424–434. https://doi.org/10.
1016/j.foodhyd.2014.10.018.
JECFA (2016). Joint FAO/WHO Expert Committee on Food Additive. Compendium of
food additive specifications. 82nd Meeting 2016. Vol 19 (Rome, Italy).
Keys, A., Grande, F., & Anderson, J. T. (1961). Fiber and Pectin in the diet and serum
cholesterol concentration in man. Proceedings of the Society for Experimental Biology
and Medicine, 106(3), 555–558.
Khorasani, A. C., & Shojaosadati, S. A. (2017). Pectin-non-starch nanofibers biocompo-
sites as novel gastrointestinal-resistant prebiotics. International Journal of Biological
Macromolecules, 94, 131–144. https://doi.org/10.1016/j.ijbiomac.2016.10.011.
Koubala, B. B., Kansci, G., Mbome, L. I., Crépeau, M. J., Thibault, J. F., & Ralet, M. C.
(2008). Effect of extraction conditions on some physicochemical characteristics of
pectins from “Améliorée” and “Mango” mango peels. Food Hydrocolloids, 22(7),
1345–1351. https://doi.org/10.1016/j.foodhyd.2007.07.005.
Laborde, J.-L., Bouyer, C., Caltagirone, J.-P., & Gérard, A. (1998). Acoustic cavitation
field prediction at low and high frequency ultrasounds. Ultrasonics, 36(1–5),
581–587. https://doi.org/10.1016/S0041-624X(97)00106-6.
Larrauri, J. A., Rupérez, P., Borroto, B., & Saura-Calixto, F. (1996). Mango peels as a new
tropical fibre: Preparation and characterization. LWT – Food Science and Technology,
29(8), 729–733. https://doi.org/10.1006/fstl.1996.0113.
Lazar, L., Talmaciu, A. I., Volf, I., & Popa, V. I. (2016). Kinetic modeling of the ultrasound-
assisted extraction of polyphenols from Picea abies bark. Ultrasonics Sonochemistry,
32, 191–197. https://doi.org/10.1016/j.ultsonch.2016.03.009.
Lopez-Avila, V., Young, R., & Teplitsky, N. (1995). Microwave-assisted extraction as an
alternatiuve to Soxhlet, sonication, and supercritical fluid extraction. Journal of
AOAC International, 79(1), 142–156.
Mahattanatawee, K., Manthey, J. A., Luzio, G., Talcott, S. T., Goodner, K., & Baldwin, E.
A. (2006). Total antioxidant activity and fiber content of select Florida-grown tro-
pical. Fruits, 54(19), 7355–7363. https://doi.org/10.1021/jf060566s.
Moorthy, I. G., Maran, J. P., Ilakya, S., Anitha, S. L., Sabarima, S. P., & Priya, B. (2017).
461
Food Research International 119 (2019) 455–461
Ultrasound assisted extraction of pectin from waste Artocarpus heterophyllus fruit
peel. Ultrasonics Sonochemistry, 34, 525–530. https://doi.org/10.1016/j.ultsonch.
2016.06.015.
Myers, R., Montgomery, D., & Anderson-Cook, C. (2002). Response surface methodology:
Process and product optimization using designed experiments (3rd). New York: Wiley.
Nagel, A., Neidhart, S., Anders, T., Elstner, P., Korhummel, S., Sulzer, T., & Carle, R.
(2014). Improved processes for the conversion of mango peel into storable starting
material for the recovery of functional co-products. Industrial Crops and Products, 61,
92–105. https://doi.org/10.1016/j.indcrop.2014.06.034.
Pandit, S. G., Vijayanand, P., & Kulkarni, S. G. (2015). Pectic principles of mango peel
from mango processing waste as influenced by microwave energy. LWT – Food Science
and Technology, 64(2), 1010–1014. https://doi.org/10.1016/j.lwt.2015.06.070.
Pardo Andreu, G. L., Delgado, R., Velho, J. A., Curti, C., & Vercesi, A. E. (2005).
Mangiferin, a natural occurring glucosyl xanthone, increases susceptibility of rat liver
mitochondria to calcium-induced permeability transition. Archives of Biochemistry and
Biophysics, 439(2), 184–193. https://doi.org/10.1016/j.abb.2005.05.015.
Rabelo, R. S., Machado, M. T. C., Martínez, J., & Hubinger, M. D. (2016). Ultrasound
assisted extraction and nanofiltration of phenolic compounds from artichoke solid
wastes. Journal of Food Engineering, 178, 170–180. https://doi.org/10.1016/j.
jfoodeng.2016.01.018.
Rafiee, Z., Barzegar, M., Ali, M., & Maherani, B. (2017). Nanoliposomal carriers for im-
provement the bioavailability of high – Valued phenolic compounds of pistachio
green hull extract. Food Chemistry, 220, 115–122. https://doi.org/10.1016/j.
foodchem.2016.09.207.
Rodrigues, E., Mariutti, L. R. B., & Mercadante, A. Z. (2013). Carotenoids and phenolic
compounds from Solanum sessiliflorum, an unexploited amazonian fruit, and their
scavenging capacities against reactive oxygen and nitrogen species. Journal of
Agricultural and Food Chemistry, 61(12), 3022–3029. https://doi.org/10.1021/
jf3054214.
Singleton, V. L., & Rossi, J. A. (1965). Colorimetry of total phenolics with acid reagents.
Journal of Enology, 16(3), 144–158.
Sogi, D. S., Siddiq, M., & Dolan, K. D. (2015). Total phenolics, carotenoids and antioxidant
properties of Tommy Atkin mango cubes as affected by drying techniques. LWT –
Food Science and Technology, 62. https://doi.org/10.1016/j.lwt.2014.04.015.
Thakur, B. R., Singh, R. K., Handa, A. K., & Rao, M. A. (1997). Chemistry and uses of
pectin ? A review. Critical Reviews in Food Science and Nutrition, 37(1), 47–73. https://
doi.org/10.1080/10408399709527767.
Videcoq, P., Garnier, C., Robert, P., & Bonnin, E. (2011). Influence of calcium on pectin
methylesterase behaviour in the presence of medium methylated pectins.
Carbohydrate Polymers, 86(4), 1657–1664. https://doi.org/10.1016/j.carbpol.2011.
06.081.
Wang, M., Fan, C., Zhao, K., Huang, B., Hu, H., Xu, X., & Liu, F. (2016). Characterization
and functional properties of mango peel pectin extracted by ultrasound assisted citric
acid. International Journal of Biological Macromolecules. https://doi.org/10.1016/j.
ijbiomac.2016.06.011.
Willats, W. G., Knox, J. P., & Mikkelsen, J. D. (2006). Pectin: New insights into an old
polymer are starting to gel. Trends in Food Science & Technology, 17(3), 97–104.
https://doi.org/10.1016/j.tifs.2005.10.008.
Zdunek, A., Kozioł, A., Pieczywek, P. M., & Cybulska, J. (2014). Evaluation of the na-
nostructure of pectin, hemicellulose and cellulose in the cell walls of pears of dif-
ferent texture and firmness. Food and Bioprocess Technology, 7(12), https://doi.org/
10.1007/s11947-014-1365-z.