Food Hydrocolloids 38 (2014) 186e192

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Food Hydrocolloids
journal homepage: www.elsevier.com/locate/foodhyd

Extraction of pectin from passion fruit peel (Passiflora edulis

f. flavicarpa) by microwave-induced heating
Fernanda L. Seixas a, *, Deise L. Fukuda a, Franciele R.B. Turbiani a, Patrícia S. Garcia a,
Carmen L. de O. Petkowicz b, Sheeja Jagadevan c, Marcelino L. Gimenes a
a
Departamento de Engenharia Química, Universidade Estadual de Maringá, Av. Colombo, 5790, Bloco D90, 87020-900 Maringá, PR, Brazil
b
Departamento de Engenharia Química, Universidade Federal do Paraná, R. XV de Novembro, 1229, 80060-000 Curitiba, PR, Brazil
c
Department of Engineering Science, University of Oxford, Parks Road, Oxford OX1 3PJ, UK

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

Article history: Pectin is a heteropolysaccharide obtained from primary cell walls of terrestrial plants, which is a very
Received 25 November 2012 important raw material for food and pharmaceutical products. Extraction of pectin from the peels of
Accepted 2 December 2013 yellow passion fruit (Passiflora edulis f. flavicarpa) under microwave-induced heating was investigated in
the present study. Three types of acids (tartaric, acetic and nitric acid) were employed as extracting
Keywords: agents. The effect of extraction time and microwave-power on yield of pectin has been studied using the
Microwave
response surface methodology. The results indicate that exposure time and microwave-power signifi-
Passion fruit peel
cantly affects the yield of pectin extraction with both nitric and tartaric acids. However, the extractions
Pectin extraction
Degree of esterification
using acetic acid were significantly affected only by the exposure time. For all scenarios, the highest
yields were obtained when the highest levels of power and time were used (628 W and 9 min). Under
these conditions, the yield of pectin obtained with nitric and acetic acids were 13 and 12.9% respectively.
Tartaric acid emerged as the best extracting agent in terms of yield (18.2%), however, the obtained pectin
exhibited low purity and low degree of esterification. Pectin extracted from passion fruit by employing
acetic and nitric acid presented better properties: high molar mass (4.625
105 for acetic acid and
4.966
105 for nitric acid), degree of esterification (64.56% for acetic acid and 64.15% for nitric acid) and
content of uronic acids (62.5% for acetic acid and 82.3% for nitric acid).
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction Pectin is a polysaccharide found ubiquitously in cell walls of all

Passion fruit (Passiflora edulis f. flavicarpa) being a good source of
vitamin C is commonly employed in juice processing. The annual
production of this juice in Brazil alone is estimated to be more than
920,158 tons in 2010 (IBGE, 2013). Such a wide-scale use of this
fruit, inevitably leads to the generation of vast quantities of the fruit
peels, which constitutes about half of the fruit mass. These fruit
peels are discarded as a major waste, causing a substantial burden
on the environment. It is therefore imperative to find adequate
disposal of these peels or means to convert the peels into useful
products (Liu, Shi, & Langrish, 2006; Pinheiro et al., 2008). Recent
studies have shown that the pericarp (integral part of the peel) of
passion fruit, even though processed and stored, could be used as
raw material for obtaining co-products in food industry, such as
dietary fiber and other bioactive compounds (Yapo, 2009a; Yapo &
Koffi, 2006).
* Corresponding author. Tel.: þ55 44 32624860.
E-mail address: fernandalini@ibest.com.br (F.L. Seixas).
plants (Carpita & McCann, 2000). This polysaccharide is mainly
composed of two moieties (i) homogalacturonan made up of (1-4)
linked a-D-galacturonic acid and (ii) rhamnogalacturonan I con-
sisting of (1-2) repeating linked, a-L-rhamnose-(1-4) and a-D-gal-
acturonic acid disaccharide. Rhamnogalacturonan I usually contains
neutral side chains of arabinan, galactan or arabinogalactan.
The ratio of esterified carboxylic acid units to total carboxylic
acid units in pectin is termed the degree of esterification (DE),
which has a major influence on gel properties of pectin. Depending
on DE, pectin is commercially divided into two major groups: high-
ester pectin, with DE higher than 50%, and low-ester pectin, with
DE lower than 50% (Thakur, Singh, & Handa, 1997).
Pectin represents a high-value functional food ingredient widely
used as gelling agent and stabilizer, particularly in jams and jellies
(Willats, Knox, & Mikkelsen, 2006). Pectin extraction is a multiple-
stage physicochemical process which involves hydrolysis and
extraction of pectin macromolecules from plant tissue, purification
of the liquid extract and isolation of the extracted pectin from the
liquid. These processes are influenced by various factors, mainly
temperature, pH, and time (Pagán, Ibarz, Llorca, Pagán, & Barbosa-

0268-005X/$ e see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.foodhyd.2013.12.001
 F.L. Seixas et al. / Food Hydrocolloids 38 (2014) 186e192
Cánovas, 2001). Usually the traditional technique requires longer
extraction time thus running the severe risk of thermal degradation
for the thermolabile materials. Conventional techniques for the
extraction of constituents are time and solvent consuming and
thermally unsafe. Keeping in pace with such requirements recent
times has witnessed the use and growth of new extraction tech-
niques with shortened extraction time, reduced solvent con-
sumption, increased pollution prevention concern and with special
care for thermolabile constituents (Luque de Castro & Garcia-Ayuso,
1998; Mandal, Mohan, & Hemalatha, 2007). Although it has been
shown that the pericarp of passion fruit can be used as raw material
for pectin isolation (Kliemann et al., 2009; Pinheiro et al., 2008;
Yapo, 2009a, 2009b; Yapo & Koffi, 2006), the extraction under
microwave heating was not investigated.
The use of microwave for extraction of constituents from plant
material has shown tremendous research interest and potential.
There are two types of microwave systems currently used: closed
extraction vessels and focused microwave ovens. The latter, used in
this work, is also named as solvent extraction, in which only a part
of the extraction vessel containing the sample is irradiated with
microwave, this system operates in atmospheric pressure (open-
vessel). The use of atmospheric pressure substantial provides ad-
vantages over pressurized vessels such as: open-vessel operation is
more suitable with thermolabile species as it uses low tempera-
tures relative to closed vessel systems; the low cost of the equip-
ment required; the absence of any requirement for cooling down or
depressurization; the ability to add reagents at any time during the
treatment, among others (Mandal et al., 2007).
In addition, conventionally, pectin is extracted from citrus peels
and apple pomace by employing strong mineral acids (May, 1990;
Rolin, 1993). The use of such strong acids in the extraction step
leads to corrosion of equipment and has deleterious effects on the
environment. The need for replacement of these extracting agents
with milder weak organic acids could be a potential means to
minimize aforementioned adverse effects. As the yield and
composition of pectins depends on the conditions used during
pectin isolation and purification (Levigne, Ralet, & Thibault, 2002;
Rolin, 1993), in this work pectins from yellow passion fruit peels
were extracted using different acids under microwave heating.
The main aim of this study was to employ two weak organic
acids, such as tartaric and acetic, and the nitric acid for extraction of
pectin from peels of yellow passion fruit under microwave heating.
The factors influencing the yield of pectin such as intensity of
electromagnetic field and exposure time were also examined. The
extracted pectin should be of high DE, purity and molecular weight
and the yield should be as high as possible.
2. Materials and methods
Samples of yellow passion fruit peel (P. edulis f. flavicarpa) were
obtained from the pulps producing industry located in Paraná,
Brazil. These fruit peel represents a waste generated during the
fruit processing operations. These peels were composed of an intact
pericarp. The commercial citrus pectin, employed for comparative
analysis was procured from Vetec P.A., Brazil. All chemical reagents
employed in this study were of analytical grade.
2.1. Preparation of passion fruit peel flour (PFF)
The fruit peels were thoroughly washed in running water and
subjected to a blanching treatment, which results in enzymatic
inactivation. For this, the peels were immersed in water at a tem-
perature of 97  C for 3 min, then, the peels were transferred to
another water bath at room temperature and maintained for
15 min. Subsequently, the peels were dried in an air-circulated oven
187
at 50  C until a constant weight was obtained. The dried peels were
then milled to 60 mesh size powdered passion fruit peel and the
resulting product, referred to as “passion fruit peel flour (PFF)”. The
passion fruit peel flour was used as raw material for pectin
extraction. The passion fruit peel flour was packaged in a poly-
ethylene bag and stored in a freezer (15  2  C) until required.
2.2. Pectin extraction
Pectin was extracted using a modified version of the method
presented elsewhere by Canteri-Schemin, Fertonani, Waszczynskyj,
and Wosiacki (2005). The extraction process was carried out in
600 mL beakers, followed by heating in a microwave oven (CCE
model M e 304). 4 g of passion fruit peel flour was added to 100 mL
of distilled water in a beaker. This was followed by addition of
100 mL of an acidic solution, with concentration adjusted so as to
maintain a final pH of 2 for the solutions. The beaker was partially
covered with a glass lid and then subjected to microwave heating
for predetermined time intervals (3, 6 and 9 min). As the extraction
system remained partially open, gradual evaporation of the solvent
was observed. In order to maintain a constant suspension con-
centration, the amount of evaporated water was replenished to the
system at regular intervals.
The suspension, still warm, was vacuum filtered in synthetic
fabrics; the retentate was discarded and the filtrate (containing the
soluble pectin) was cooled to 4  C. To isolate the soluble pectins
from the filtrate, the extracted liquid was slowly added under
magnetic stirring to two volumes of absolute ethyl alcohol, both
maintained at 4  C. This mixture was stirred for 10 min, after which
it was allowed to rest for 30 min to facilitate the flotation of the
pectin. The pectin thus obtained, was separated by vacuum filtra-
tion on a filter paper. The extracted pectin in a gel form was
immersed in absolute ethyl alcohol for about 12 h and then was
partially dehydrated by immersion in acetone for a few minutes.
This was followed by drying pectin in an air-circulated oven at 40  C
until constant weight was obtained (approximately five hours). The
resulting material was milled to dry powdered pectin. The extrac-
tion process of pectin is schematized in Fig. 1.
2.3. Experimental design
Response surface methodology was used to determine the op-
timum condition for pectin extraction from passion fruit peel flour.
In order to evaluate the effect that the variables extraction time (tEx)
and microwave power (P) present on the yield of pectin extracted
(response) a complete factorial experimental design 22 was elab-
orated with the insertion of a central point. Experiments in the
centre of the design were performed in order to make the esti-
mation of pure error possible. The variable extraction time was
evaluated at the levels 3, 6 and 9 min and the microwave power
was evaluated at levels 356, 450 and 627.9 W. The pH of the solu-
tion was maintained constant (2.0) for the three kinds of acids
studied. The complete design consisted of 4 experiments for each
type of acid examined and three replicates in center point (Table 1).
All the tests were conducted in duplicate at random. The t-Student
test was performed with a significance level of 5%. For data analysis
was used the software Statistica 10.
2.4. Degree of esterification
The degree of esterification (DE) of pectin samples were deter-
mined by potentiometric titration, as described by Bochek,
Zabivalova, and Petropavlovskii (2001). The percentage of gravi-
metric yield of pectin was calculated from the ratio of the mass of
dried pectin extracted and the mass of flour used as raw material.
188 F.L. Seixas et al. / Food Hydrocolloids 38 (2014) 186e192

solution, with respect to changes in solute concentration) was

determined using five concentrations in the 1e0.2 mg ml1 range
Passion fruit peel flour
(PFF)
using a Waters 2410 differential refractometer. The average molar
Distilled water mass (Mw) and polydispersity index were determined from HPSEC-
Suspension
MALLS data using Wyatt Technology ASTRA software.
(4 g PFF + 100 mL distilled Acid solution (100 mL)
water, (acetic, tartaric or nitric acid) 2.6. Monosaccharide composition
Ratio solid: liquid of 1:25 (g/mL))

2.6.1. Acidic monosaccharides content

pH = 2
The determination of uronic acid was performed by the method
Microwave heating described by Blumenkrantz and Asboe-Hansen (1973), with gal-
(Controlled variables: time and
power extraction)
acturonic acid as a standard solution, taken at concentrations of
10e100 mg/mL and the absorbance read at 520 nm. Analyses were
performed in quadruplicates.
Insoluble
Filtration residue
2.6.2. Neutral monosaccharides
Pectin solubilized The samples were hydrolyzed with 2 M trifluoroacetic acid for
Flotation Pectin in alcohol 5 h at 100  C (Biermann, 1989). The monosaccharides were reduced
(Ratio pectin solution:alcohol with sodium borohydride for 16 h at 4  C (Wolfrom & Thompson,
1:2 mL/mL)
1963b). Subsequently, samples were treated with strong acid
cation resin and methanol as previously described (Vriesmann,
Rinsing with Teófilo, & Petkowicz, 2011). The alditol formed were acetylated
ethanol Filtration
with pyridineeacetic anhydride (1:1, v/v, 16 h, at 25  C) (Wolfrom &
Pectin gel Thompson, 1963a). The alditol acetates formed were extracted with
Drying at 40 °C chloroform and submitted to successive treatments with copper
sulphate and 5% distilled water for elimination of pyridine. The
alditol acetates were analyzed by gaseliquid chromatography (GLC)
Dry pectin using a (Trace GC Ultra, Thermo Electron Corporation) equipped
with a DB-225 capillary column (0.25 mm
30 m). The tempera-
Fig. 1. Flow diagram for the extraction of pectin. tures of injector and flame ionization detector (FID) were main-
tained at 250  C and 300  C, respectively. The oven temperature
was programmed from 100  C to 215  C at a heating rate of 40  C/
The data were statistically analyzed by applying the Tukey test with min. Helium was used as carrier gas at a flow rate of 1.0 mL/min.
a significance level of 5% using the software Statistica 10.
2.7. Morphology
2.5. High performance size exclusion chromatography
In order to visualize the morphology of the samples of passion
The extracted pectin samples were analyzed by high perfor- fruit peel flour, scanning electron microscope (Shimadzu SS - 550,
mance size exclusion chromatography (HPSEC) coupled to a Superscan, software Superscan SS-550) image were taken before
refractive index (RI) and a Wyatt Technology Dawn-F multi-angle and after the extraction process. The samples were adhered to a
laser light scattering (MALLS) detector. The RI detector provides support with the use of a double-sided conductive carbon tape and
data proportional to the concentration of pectin, whereas the then metallized with gold to ensure electrical conductivity to the
MALLS furnishes data on the molar mass. Four ultrahydrogel col- observed surface.
umns e 120, 250, 500 and 2000 were used with exclusion limits of
5
103, 8
104, 4
105 and 7
106, respectively. A 0.1 M NaNO2 3. Results and discussion
solution containing 200 ppm NaN3 was employed as an eluent. The
samples were dissolved at a concentration of 1.5 w/v in the eluent. 3.1. Extraction
Before analysis all samples were filtered through cellulose acetate
membranes with pore size of 0.22 mm. The analyses were carried The experimental yields of pectin obtained for extraction using
out at 25  C. For the average molar mass (Mw) calculation, the dn/dc three different acids (nitric, acetic and tartaric) are presented in
value (the refractive index increment of the solventesolute Table 1. Was adjusted a factorial model which analyzed the in-
fluences of factors tEx, P and the interaction tEx
P. Multiple
Table 1
regression coefficients are shown in Table 2. The results showed
Yield of pectins extracted passion fruit peels under microwave heating using nitric that for extractions carried out with nitric acid and tartaric, both
acid, acetic acid and tartaric acid. variables (tEx and P) as well as their interactions (tEx
P) was
Variable (coded level) a
Yield (%)
significant by t-Student test at a significance level of 0.05. For the
case of extractions performed with acetic acid results suggest that
Power (W) Time (min) Nitric acid Acetic acid Tartaric acid
only the extraction time significantly affects the extraction yield. In
356 (1) 3 (1) 9.1 9.4 15.3 this case, the power of the microwave is not very important. Thus,
356 (1) 9 (1) 9.9 12.7 18.2
the extraction process using acetic acid may be conducted at the
628 (1) 3 (1) 9.2 11.4 16.0
628 (1) 9 (1) 13.0 12.9 30.3 lowest level of radiation (356 W) with no damage as the yields
450 (0) 6 (0) 10.3 12.0 17.0 obtained.
450 (0) 6 (0) 10.9 11.8 16.8 Figs. 2e4 show the response surfaces coded levels obtained
450 (0) 6 (0) 11.0 12.4 16.4 from the fitted model for the three acids analyzed. The quality of
a
Based on passion fruit peel flour. the model can be observed by the high R2 values obtained
 F.L. Seixas et al. / Food Hydrocolloids 38 (2014) 186e192 189

Table 2
Coded regression coefficients, standard error and p values for the model built.

Factor Acetic acid Nitric acid Tartaric acid

Coeff Std. Err. p Coeff Std. Err. p Coeff Std. Err. p

Interc. 11.80* 0.163 9.0 E-6 10.49* 0.170 9.0 E-6 17.78* 0.535 6.0 E-5
P (W) 1.10 0.432 8.4 E-2 1.60* 0.450 3.8 E-2 9.15* 1.414 7.5 E-3
tEx (min) 2.40* 0.432 1.2 E-2 2.30* 0.450 1.5 E-2 5.85* 1.414 2.6 E-2
P
tEx 0.90 0.432 1.3 E-1 1.50* 0.450 4.5 E-2 8.45* 1.414 9.4 E-3
Adj. R2 0.93 0.94 0.96

*Significative at significance level of 0.05.

(see Table 2). Beyond what we can assume that normality, inde-
pendence and randomness of the residuals were satisfied.
From these results it is possible to observe that for all acids
analyzed the highest yields were obtained when the highest field
strength (628 W) and exposure time (9 min) were used (Figs. 2e4).
Tartaric acid was the best extracting agent (Table 1), with yields
between 15.32 and 30.29%. For acetic acid, yields remained between
9.43 and 12.91% and for nitric acid between 9.5 and 13.1%. The re-
sults showed that not only concentration, but also acid type influ-
enced the extracted pectin yields (Yapo, 2009a, 2009b) and that the
use of tartaric acid in place of strong mineral acids is an efficient
alternative as the former performed better in terms of extraction
yield. These results are in accordance to study conducted by Yapo
(2009a, 2009b), wherein, 3e14% yields were obtained for extrac-
tions carried out by using citric, nitric and sulfuric acids at different
concentrations (10 mM and 30 mM) and pH (1.8 and 2.5). Similar
pectin yields (8e13.1%) were obtained by Fishman, Chau, Hoagland,
and Hotchkiss (2006), while studying the effect of microwave-
assisted extraction under pressure on lime flavedo, albedo and
pulp. The extractions were carried out at 630 W of power in a so-
lution of HCl (pH 2.0) with heating times ranged from 1 to 10 min.
However, although the tartaric acid has afforded the highest
yields, pectin extracted with this agent had some undesirable
qualities, such as: low molar mass and lower uronic acid content.
On the other hand, pectin extracted with acetic acid showed a high
molar mass and high uronic acid content. Therefore, as they are
both mild acids further studies are needed to explain what are the
mechanisms of action, during the extraction process, of such acids
and thus to understand the differences in the properties of pectin
obtained.
Preliminary extraction studies performed on a condensing
thermostatic bath (conventional process), conducted at pH 2.0,
90  C and 40 min, resulted in 19.40%, 10.20% and 12.94% yields for
extractions carried out with tartaric acid, acetic acid and nitric acid
respectively (results not shown). Comparing these results with
those from Table 1, an increased yield of pectin was observed for
extractions conducted under microwave heating, especially while
employing organic acid as an extraction medium. This effect may be
due to the changes occurring in plant tissues when subjected to
microwaves.
The electromagnetic field energy is converted to heat, especially
in polar substances, causing formation of intense vapors inside the
capillary porous structure of the plant material, thereby leading to
modification in their physical properties (Kratchanova, Pavlova, &
Panchev, 2004).
In the present study, an increase in temperature from micro-
waves may have caused rupture of the parenchymal cells of the
plant material. The damage to the plant tissue increased with
increasing intensity of the microwave field, which is explained by
an increase in intracellular spaces. The images of scanning electron
microscopy for the passion fruit peel flour, before (a) and after (b)
undergoing the extraction process can be seen in Fig. 5. It can be
clearly seen that extraction under microwave heating promotes an
increase in capillary porosity of the passion fruit peel, so the cell
will split and the pectin and other inclusion can release itself.

Fig. 2. Response surface showing the effect of extraction time (coded values) and Fig. 3. Response surface showing the effect of extraction time (coded values) and
power (coded values) on yield of pectin for extractions carried out with acetic acid. power (coded values) on yield of pectin for extractions carried out with nitric acid.
190 F.L. Seixas et al. / Food Hydrocolloids 38 (2014) 186e192

Table 3
Monosaccharide composition and DE of pectins extracted from passion fruit peels
using acetic acid, tartaric acid and nitric acid compared with the commercial citrus
pectin.
b
Monosaccharide Acetic Tartaric Nitric Commercial
(%) acid acid acid

Rhamnose 4.0 5.9 2.6 3.1

Fucose 0.5 0.6 0.3 0.1
Arabinose 9.5 8.1 4.1 6.8
Xylose 2.5 2.5 1.6 0.5
Mannose 1.8 1.7 0.7 0.9
Galactose 6.8 9.2 3.6 12.7
Glucose 12.4 13.5 4.8 0.0
Uronic acid 62.5 58.5 82.3 75.8

DEa 64.56 50.00 64.15 70.0

(1.90) (1.48) (1.65) (0.55)
a
Mean (standard deviation) (3 repetitions).
b
Neutral monosaccharides were determined by GLC and uronic acid content was
obtained by colorimetric method.

Fig. 4. Response surface showing the effect of extraction time (coded values) and
power (coded values) on yield of pectin for extractions carried out with tartaric acid.
Zhongdong, Guohua, Yunchang, and Kennedy (2006) extracted
pectin from orange skin and also observed that microwave radia-
tion has the stronger destructive effect on the organization struc-
ture of orange skin, and the swelling effect of the microwave event
forces of the cells to split.
Thus, if one compares the extraction process under microwave
heating with the conventional extraction process it is observed that
in addition higher yields it is possible to get significant energy
savings, since the conventional process lasts for about an hour,
while microwave process has duration of only a few minutes.
3.2. Characterization of pectin
Pectin extracted under the conditions that generated the high-
est yield (9 min and 628 W), for the three types of acid, were
characterized and compared with commercially available citrus
pectin (Vetec) for its degree of esterification, chemical composition
and molar mass distribution.
3.2.1. Degree of esterification
Table 3 enlists the values of the degree of esterification (DE) of
pectins isolated from passion fruit peels which were in the range of
50.00e64.56%. The DE values were influenced by the kind of acid
used in the extraction. The highest DE were observed for pectins
obtained with acetic acid (64.56%) and nitric acid (64.15%) while the
extraction with tartaric acid afforded pectins with the lowest DE
(50.00). The DE values for pectins extracted with acetic acid and
nitric acid were close to that found for commercially available citrus
pectin (70%).
The pectins obtained in the present work had a medium to high
degree of esterification (above 50%) and hence can be considered to
be of great economic interest, as per the conventional classifica-
tions (Thakur et al., 1997). It is of interest to note that unlike con-
ventional methods of extraction, microwave extraction, produces
high DE pectin (Fishman et al., 2006).
Pinheiro et al. (2008) extracted pectins from passion fruit peel
using citric acid at different concentrations and extraction times.
They obtained pectins with DE ranging from 27.52% to 78.59%. Using
a surface response methodology these authors found the satisfac-
tory condition for extraction of high DE pectin with citric acid
(0.086% w/v citric acid for 60 min). The extraction with acetic acid
for 9 min under microwave heating resulted in a pectic fraction with
DE 64.56. Yapo (2009b) used pure lemon juice and citric acid to
extract pectins from passion fruit peel at 80  C for 90 min and ob-
tained polysaccharides with DE 52e73%. In the present work, high
DE pectins with DE w65% were isolated from passion fruit peel
using lower times of extraction (9 min), showing the advantage of
this method of extraction when compared with the traditional ones.
3.2.2. Monosaccharide composition
The monosaccharide composition of pectins extracted from
passion fruit peels with different acids, compared with the com-
mercial citrus pectin is shown in Table 3. Since the commercial

Fig. 5. Scanning electron microscopy for the passion fruit peel flour before (a) and after (b) extraction under microwave heating (magnification 200
).
 F.L. Seixas et al. / Food Hydrocolloids 38 (2014) 186e192 191

pectin is standardized using glucose, the glucose content of the

sample (w26%) was not considered in the monomeric composition
of the polymer. The pectins contain uronic acid as the main
component (58.5%e82.3%). Among the neutral monosaccharides,
glucose, galactose, arabinose and rhamnose were found in higher
amounts. Galactose, arabinose and rhamnose arise from rhamno-
galacturonan region. The commercial sample showed a greater
level of galactose (12.7%) compared to samples obtained experi-
mentally (3.6%e9.2%).
Pectins extracted with nitric acid and acetic acid which had the
highest DE also displayed the highest uronic acid contents, 82.3%
and 62.5%, respectively. These levels of uronic acid are higher than
those found by Yapo (2009b) for pectins extracted from passion
fruit peel using pure lemon juice and citric acid which ranged from
63.8% to 78.3%. However, lower uronic acid content (58.5%) was
observed for pectins extracted with tartaric acid. As established by
FAO and EU, a minimum of 65% of galacturonic acid is required to be
Fig. 6. Curves of differential weight fraction as a function of molecular weight of
considered as pectin (Willats et al., 2006). Thus, the poly- pectins extracted from passion fruit peels under microwave heating using nitric acid,
saccharides extracted with nitric and acetic acid from passion fruit acetic acid and tartaric acid, compared with the commercial citrus pectin.
peel and commercial citrus pectin (Vetec) can be classified as
pectin. Value below the required standard was found for pectin weight fraction) is contained in any molar mass interval. It is
extracted from passion fruit peel with tartaric acid. possible to observe that the pectins obtained by extracting with
The ratio of uronic acid to rhamnose, an indicator of the pro- nitric acid present a sharp peak, with the narrowest distribution, in
portion of homogalacturonan and rhamnogalacturonan I in the accordance with its lower Mw/MN. By the other side, pectin
polymer, remained between 20 and 32 during extractions with extracted with acetic acid showed the wider distribution of mole-
acetic and nitric acid, respectively. The results suggest that these cules, between 2
104 g/mol and 2
106 g/mol.
pectin samples consist mainly of linear regions of galacturonic acid. Comparing the organic acids used in this work, it is noteworthy
These results are in accordance to the data recently published for that the curve for the pectin extracted with tartaric acid was shifted
pectins extracted from yellow passion fruit peel where galacturonic to lower molar mass values. This is due to the fact that tartaric acid
acid to rhamnose ratios ranged from 14 to 35 (Yapo, 2009a). has two terminal carboxyl groups, thus, its higher hydrolytical
However, for pectin extracted with tartaric acid, the uronic acid to power was greater than that of acetic acid which has only one
rhamnose ratio was 10. terminal carboxylic. Therefore, despite the use of tartaric acid
provide higher yields, your higher hydrolytical power degrades the
pectin extracted.
3.2.3. Molar mass
The pectins were analyzed by high-performance size-exclusion
4. Conclusions
chromatography (HPSEC) equipped with multi-angle laser light
scattering (MALLS) and refractive index (RI) detectors. The results
The greatest extraction yields in pectin were obtained when
of dn/dc, average molar mass (Mw) and polydispersity index (Mw/
highest field strength and exposure time was employed. The type of
MN) calculated from HPSEC-MALLS are given in Table 4. The highest
acid used also affected the yield of extraction and the composition
Mw values were found for pectins extracted with nitric acid and
and molar mass of pectin obtained. The hydrolytic power of tartaric
acetic acid, 4.966
105 g/mol and 4.625
105, respectively. The
acid makes it more active for extraction and also more active for
pectin extracted with tartaric acid had the lowest Mw,
degrading pectin than the other acids investigated. By using the
2.298
105 g/mol, which was lower than that calculated for the
response surface analysis, we can conclude that extraction time
commercial sample (3.073
105 g/mol). These results are similar to
significantly affects the yield of pectin obtained using all acids. The
those found by Fishman et al. (2006) for pectin extracted from lime
microwave power significantly affects the yield only in the case of
under 3 min of microwave heating (3.1e5.15
105 g/mol).
extractions carried out with nitric and tartaric acids. The pectin
The polydispersity index (Mw/MN) of the polymers ranged from
extracted from the peels of passion fruit exhibited medium to high
2.492 for pectin extracted with acetic acid to 1.250 for pectin
degree of esterification (50.00%e64.56%). Pectins obtained by the
extracted with nitric acid. The highest Mw/MN for pectin extracted
use of acetic acid and nitric had a yield of approximately 13.0% and
with acetic acid indicating a broader range of polymer size distri-
showed the highest DE, molar mass and uronic acid contents.
bution in this sample.
Highest yields were obtained the use of tartaric acid (30%), however,
The differential molar mass distribution for pectins obtained
the extracted pectin had some undesirable qualities, such as: low
with different acids under microwave heating is shown in Fig. 6. It
molar mass and lower uronic acid content (58.5%) and DE (50%).
is possible to observe that the samples shown a uniform distribu-
tion of sizes. The curves show how much material (differential
Acknowledgment
Table 4
Results from HPSEC-MALLS for pectins extracted from passion fruit peels under The authors gratefully acknowledge the Conselho Nacional de
microwave heating using nitric acid, acetic acid and tartaric acid, compared with the Pesquisa e Desenvolvimento Científico e Tecnológico (CNPq) of
commercial citrus pectin. Brazil for the financial support.
Pectin sample dn/dc Mw (g/mol) Mw/MN

Acetic acid 0.127 4.625
105 2.492  0.026

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