Food Research International 113 (2018) 327–350

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Food Research International

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

Review

Extraction, purification and characterization of pectin from alternative T

sources with potential technological applications
⁎
Florina Dranca , Mircea Oroian
Faculty of Food Engineering, Stefan cel Mare University of Suceava, Romania

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

Keywords: Pectins are defined as a group of widely distributed plant cell wall polysaccharides that contain galacturonic acid
Pectin linked at both the 1 and 4 positions. The wide use of pectin as an ingredient which imparts rheological and
Sources textural properties to various food products and the development of applications beyond the food industry have
Purification brought about its increase in production and influenced research towards alternative sources and improving the
Fractionation
overall isolation process of pectic polysaccharides. In this context, this paper aims to give a complete perspective
Composition
on the current state of pectin research by mainly focusing on recent research on the extraction of pectin from
Analysis
other feasible sources, on the post-extraction stages of pectin recovery from plant materials (purification and
fractionation), and, finally, on the advancements in the study of the physical, chemical, rheological, and func-
tional properties of pectin.

1. Introduction of pectins, such as galacturonan methoxylation, galacturonic acid

Fruits, vegetables, and other plant-based foods contain a wide range
of dietary components essential to the human body and are rich in
bioactive phytochemicals that may provide desirable health benefits
beyond basic nutrition (Liu, 2013). Plant foods are particularly im-
portant as a source of dietary carbohydrates, providing almost all of the
carbohydrate intake, and therefore much of the energy in the adult diet
(Lovegrove et al., 2015). Depending on the functional role, plant car-
bohydrates can be divided into two classes: storage carbohydrates
(particularly starch) and cell wall carbohydrates. Given the fact that in
plants starch-derived polysaccharides outweigh all others, the re-
mainders are collectively known as non-starch polysaccharides (NSPs)
(BeMiller, 1996). NSPs constitute the major fraction of the plant cell
wall in association and/or substituted with other polysaccharides, and
they cover a great variety of biological functions and chemical struc-
tures (Kumar, Sinha, Makkar, de Boeck, & Becker, 2012). Structurally,
NSPs are polysaccharides that contain up to several hundred thousand
monosaccharide units joined through glycosidic linkages. The major
plant cell wall NSPs are cellulose, hemicelluloses, and pectins.
Pectins represent a group of structurally heterogeneous poly-
saccharides widely distributed in primary cell walls and the middle
lamella of higher plants (Luo et al., 2017). Pectic polysaccharides are
vital structural components of plant cell walls, and they are often as-
sociated with other cell wall polysaccharides such as cellulose and
hemicelluloses. The diverse structural and macromolecular properties
content, the composition of neutral sugars, and molecular weight, are
dependent on the pectin source and set the basis for multiple food and
non-food applications of this complex polysaccharide (Yoo et al., 2012).
In the food sector, traditional usage as a gelling agent, thickening agent,
and stabilizer is being complemented by the emerging utilization of
pectin as a fat replacer and health-promoting functional ingredient
(Ciriminna, Fidalgo, & Delisi, 2016; Min, Bae, Lee, Yoo, & Lee, 2010;
Peng, Xu, Yin, Huang, & Du, 2014). Non-food applications include the
use in the medical and pharmaceutical industries, where the health-
promoting benefits and bioactivities of pectin have shown potential for
biomedical applications including drug delivery, tissue engineering,
and wound healing, as reviewed previously by Munarin, Tanzi, and
Petrini (2012). Each of the above-mentioned applications begins with
the isolation of pectin from the plant material. Generally, pectin is
isolated from by-products of agro-foods. Pectin production dates back
to the early 1900s when German producers of apple juice started to
cook dried apple pomace, the main by-product of juice processing, and
sold the extracted pectin as a gelling agent (Ciriminna, Chavarría-
Hernández, Inés Rodríguez Hernández, & Pagliaro, 2015). Apple po-
mace and citrus peel remain the main sources for the production of
commercial pectins, although other sources were considered due to
rising demand and growing interest in valorizing side streams to obtain
pectins with diverse functional properties (Christiaens et al., 2015;
Müller-Maatsch et al., 2016). Progress was also made in the extraction
technologies with the emergence of novel and effective techniques that

⁎
Corresponding author.
E-mail address: florina.dranca@fia.usv.ro (F. Dranca).

https://doi.org/10.1016/j.foodres.2018.06.065
Received 20 February 2018; Received in revised form 25 June 2018; Accepted 28 June 2018
Available online 30 June 2018
0963-9969/ © 2018 Elsevier Ltd. All rights reserved.
F. Dranca, M. Oroian
inclined toward a cleaner process (Yang, Wang, Hu, Xiao, & Wu, 2018).
With an increasing number of studies that propose new by-products
and agricultural waste as sources for pectin extraction (Morales-
Contreras, Rosas-Flores, Contreras-Esquivel, Wicker, & Morales-Castro,
2018; Sabater, Corzo, Olano, & Montilla, 2018; Xu et al., 2018), a re-
view of the potential for the capitalization of these raw materials is
demanded. One other main objective of this review is to assess the
methods applied for the purification and fractionation of the extracted
pectin prior to analyzing its composition and properties. It is important
to be noted that the characterization of pectins extracted from different
sources is a target point of this paper as it is rarely thoroughly examined
in other reviews.
2. Chemistry and function
Although the plant cell wall was first observed and defined by
Robert Hooke (1665) many centuries earlier, the knowledge regarding
its architecture has increased considerably since the 1900s. Detailed
characterizations of the structure of the plant cell wall were presented
by Preston (1975) and Clarke and Knox (1979), who described the
deposition of cell walls in three layers, primary wall, middle lamella,
and secondary cell wall. An oversimplified sketch of the plant cell wall,
adapted from McCann and Roberts (1992) and modified, is presented in
Fig. 1. Concerning the structural components, the growing plant cell
wall consists of a mixture of polysaccharide and polyuronide compo-
nents (Jansen & Jang, 1960; Ponce, Ziegler, Stortz, & Sozzi, 2010). Both
earlier determinations and subsequent studies agreed that the main
components are cellulose, hemicelluloses, and pectin (Mankarios, Hall,
Jarvis, Threlfall, & Friend, 1980; Houwink & Roelofsen, 1954;Thimann
& Bonner, 1933). Because of their multiple interaction properties,
pectins are considered key structural elements of the plant cell wall
architecture. An in-depth understanding of the biological function
should cover all the particularities related to the chemistry of pectin, as
its structural complexity imparts unique and diverse physical and bio-
chemical properties. The chemistry, biosynthesis and functions of
pectin have been reviewed multiple times recently, and therefore this
section will be a summary of current knowledge.
Prior to reporting on the progress made in the study of pectin
chemistry and biosynthesis, it is essential to emphasize that the term
‘pectin’ does not refer to a single structural cell wall polymer, but it is
rather attributed to a family of plant cell wall polysaccharides and/or
glycan domains that contain galacturonic acid residues linked at both
the 1 and 4 positions (Atmodjo, Hao, & Mohnen, 2013). To date, all
research suggests that, similar to other plant cell wall polysaccharides,
pectin is synthesized in the Golgi apparatus. Pectin synthesis is a
complex process, involving a large number of unique enzymes as cat-
alysts in the formation of each glycosidic linkage and in the modifica-
tion of some glycosyl residues in pectic chains. The biosynthetic en-
zymes required for the process include glycosyltransferase (Bouton
et al., 2002; Scheible & Pauly, 2004), methyltransferase (Mouille et al.,
2007), acetyltransferase (Pauly & Scheller, 2000),
Fig. 1. Structure of primary plant cell wall (adapted from McCann & Roberts (1992)).
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Food Research International 113 (2018) 327–350
galacturonosyltransferase (Sterling et al., 2006), glucuronosyl-
transferase (Iwai, Masaoka, Ishii, & Satoh, 2002), arabinosyltransferase
(Harholt, 2005), and xylosyltransferase (Jensen et al., 2008). The me-
chanics of pectin synthesis have been extensively reviewed by Scheller,
Jensen, Sørensen, Harholt, and Geshi (2007), Mohnen (2008), Caffall
and Mohnen (2009), Sila et al. (2009), Harholt, Suttangkakul, and Vibe
Scheller (2010), and Atmodjo et al. (2013), and therefore will not be
further discussed.
Many structurally different regions were identified in the composi-
tion of pectins, and of these three classes of pectic polysaccharides have
been extensively studied in primary cell walls: homogalacturonan (HG),
rhamnogalacturonan I (RG-I), and rhamnogalacturonan II (RG-II)
(Christiaens et al., 2016). The unsubtituted HGs are linear homo-
polymers consisting of α-(1-4) linked D-galacturonic acid (GalA) re-
sidues. HGs are known to represent the ‘smooth’ region of pectin, while
RG-I, a segment rich in neutral sugars, is considered the ‘hairy’ region
(De Vries, Voragen, Rombouts, & Pilnik, 1981). RG-I was found to
possess a backbone containing diglycosyl repeats of [→2)-α-L-Rhap-
(1→4)-α-D-GalpA-(1→] that has various side chains attached to O-4 of
the L-rhamnosyl residues (Darvill, McNeil, Darvill, & Albersheim, 1980;
Lau, McNeil, Darvill, & Albersheim, 1985; Willats, Mccartney, Mackie,
& Knox, 2001). Studies of the branched RG-I regions of apple pectin
resulted in the isolation of xylogalacturonan (Schols, Bakx, Schipper, &
Voragen, 1995), while apiogalacturonan, another HG analogue, was
determined in the cell wall of Lemna minor (Hart & Kindel, 1970). A
structure which is often described as a stretch of the HG backbone was
found for RG-II, a complex polysaccharide yielding different mono-
saccharides, including the rarely observed sugars apiose, 2-O-methyl-
xylose, and 2-O-methylfucose (Darvill, McNeil, & Albersheim, 1978).
The basic structure of pectin and the structural variations observed
in pectin segments have been reviewed by many authors including
Willats, Knox, and Mikkelsen (2006), Voragen, Coenen, Verhoef, and
Schols (2009), Kumar et al. (2012), Zhang, Xu, and Zhang (2015), and,
more recently, Chan, Choo, Young, and Loh (2017). A schematic re-
presentation of the composition of pectin elements, as proposed by Hilz
(2007), completed by including the representative side chains of RG-I
(Caffall & Mohnen, 2009), is given in Fig. 2. Some of these pectin ele-
ments show little change in the conformation of the polysaccharide
chains in different plant species, while the well-preserved RG-II is the
only pectic element that is not structurally diverse (O’Neill, Ishii,
Albersheim, & Darvill, 2004). This observation is broadly supported by
many lines of scientific evidence, including the recent study of the
polysaccharides from Citrus unshiu peel, where Park, Park, Do Hong,
Suh, and Shin (2017) concluded that the structure of the purified RG-II
was very similar to the one presented in Fig. 2. On the other side, the
detailed structure of RG-I from various plant materials is often very
distinct and similar to the conformation presented in Fig. 2, mainly due
to the high variability of its side chains. Accordingly, non-ramified RG-I
chains were found in the key areas for cell adhesion of the tomato
pericarp tissue during its development (Guillon et al., 2017), while a
similar type I rhamnogalacturonan backbone with branches of β-1,4-D-
F. Dranca, M. Oroian
Fig. 2. Schematic representation of the composition of pectin structural ele-
ments (Caffall & Mohnen, 2009; Hilz, 2007).
galactan side chains occasionally substituted with α-L-Araf was iden-
tified in pumpkin residue (Zhao et al., 2017). When compared to RG-I
isolates from pumpkin residue, ginseng pectin displayed a greater
variety of RG-I domains. From ginseng pectin Yu et al. (2010) isolated
five RG-I domains, all containing galacturonic acid, rhamnose, ga-
lactose, and arabinose as main components. Four of these had side
chains of type I and probably type II arabinogalactans, and one pre-
sented 4-O-methyl-β-D-glucuronic acid residues at non-reducing
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Food Research International 113 (2018) 327–350
terminals.
A particularity in the structure of pectic substances is the ester-
ification by methyl groups (at C-6) and/or acetyl groups (at O-2 and/or
O-3) of galacturonic acid residues on the continuous poly-(GalA) chain
of HG (Yapo & Koffi, 2013). The overall degree of substitution is known
as degree of methylation (DM) and acetylation (DAc), respectively. The
degree of methylation, based on which pectins are divided into two
categories – high-methoxyl pectins (HMP, DM > 50%) and low-meth-
oxyl pectins (LMP, DM < 50%) – is an important parameter in choosing
the most suitable pectin application (Łȩkawska-Andrinopoulou,
Vasiliou, Georgakopoulos, Yialouris, & Georgiou, 2013).
Within the pectic polysaccharides group, several individual com-
ponents have been identified and characterized, yet the assembly me-
chanism of these components in the plant cell wall is the subject of
continuous research. Moreover, knowledge of the interactions estab-
lished between pectic polysaccharides and the interconnections of
pectin molecules with other cell wall components is relatively limited.
It is generally accepted that these interactions are particularly built
upon cross-links between macromolecular components of the cell wall
and intercellular adhesion. A number of covalent and non-covalent
interactions, which include ionic bridges, ferulic acid linkages, borate
esters and uronyl esters, are considered to be involved in intra- or in-
termolecular linkages. A comprehensive analysis of the formation,
mechanisms, reaction conditions, and the macromolecular functionality
of the pectic polysaccharide cross-links (Fig. 3) can be found in the
review published by Zaidel and Meyer (2012). Cross-linking of pectic
polysaccharides is believed to have a major influence on both the
physical and macromolecular properties of plant materials and, con-
sequently, it impacts their processing and quality. Alongside cross-
linking, pectin biosynthesis, conversion reactions (enzymatic and non-
enzymatic), and the solubility property of pectic polysaccharides, are
considered key mechanisms that dictate the structure-function re-
lationships of pectin. A rather common principle of research on the
chemistry of pectin is that the structural features govern its functional
properties. Structure-function relations can be studied in the context of
pectin’s functionality within plant cell walls, and from the perspective
of selecting a suitable industrial application based on functional prop-
erties and physiological benefits. The review previously published by
Sila et al. (2009) consists of a comprehensive discussion involving all
the aspects regarding structure-function relationships, including their
importance for the continuously evolving analysis methodology of
pectins.
3. Sources for pectin production: the potential of other vegetable
wastes
Different types of polysaccharides and their derivatives recovered
from plants and vegetables are currently used to obtain biopolymers
with multiple uses in several distinct areas such as the health care, food,
and polymer processing industries. In the food industry, the main use
for the extracted pectin (labeled in the European Union as E440) is as a
gelling agent in the production of fruit-based products and fillings for
bakery and confectionary products. Pectin is also applied in food pro-
duction as a thickening, stabilizing, and emulsifying agent. From the
point of view of these applications, the most frequently exploited
structure-function relationship is the one between the methoxylation of
the galacturonic acids in pectin backbone and pectin gelation. HMP
(DM above 50%) form gels through hydrophobic interactions and hy-
drogen bonds under suitable conditions: pH≤3.5 and high sugar con-
tent (> 55%) (Kastner et al., 2014). On the other side, the gelation
process of LMP (DM < 50%) is governed by the cross-linking of HG
chains via Ca2+ bridges, occurring after the addition of calcium ions to
the pectin solution (Han et al., 2017). All the applications of pectin in
the industry begin with the isolation of pectin from the plant material.
At the present time, commercial production of pectin is limited to two
major sources, apple pomace and citrus peel. Both extraction sources
F. Dranca, M. Oroian
Fig. 3. Pectic polysaccharides cross-linking: (A) calcium bridges, (B) uronyl ester, (C) ferulic acid oxidation, and (D) RG-II – borate ester (adapted from (Zaidel &
Meyer, 2012)).
represent by-products of juice manufacturing operations. Since the first
commercial production of liquid pectin from apple pomace, docu-
mented in 1908 in Germany, the industry has seen rapid growth in
Europe and North America. Nowadays, the largest part of commercially
available pectin originates from citrus peel (85.5%), and only a small
proportion is covered by extraction from apple pomace (14.0%) and
sugar beet pulp (0.5%) (Ciriminna et al., 2015). Hence, the production
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Food Research International 113 (2018) 327–350
is centered in the European region and in citrus-producing countries of
South America (Bhatia, Sharma, & Alam, 2016).
Wastes resulting from apple and citrus processing are traditionally
the main sources of commercial pectin. Compared to citrus peel, apple
pomace has the disadvantage of a lower content of pectin. The differ-
ence in pectin content between apple varieties has been investigated
along the years, and led to the understanding that winter (or late-
F. Dranca, M. Oroian
season) varieties give the best pectin quality and extraction yields
(National Institute of Industrial Research Board, 2010). The pectin
content of dried pomace obtained from the commercial Granny Smith
apple was determined by Constenla, Ponce, and Lozano (2002), who
reported that the extraction in nitric acid solution resulted in a max-
imum pectin yield of 4.2%. A newer study by Kumar and Chauhan
(2010) aimed to characterize the pectin from two different varieties of
apple, Royal and Golden, cultivated in Himachal Pradesh, India. For
both varieties maximum extraction yields of pectin from pomace were
obtained by using diluted citric acid and were as follows: 16.65% for
Royal variety and 18.79% for Golden variety. As the harvest period for
Royal variety is mid-late season, while Golden apples are a late-season
variety, the results of this study confirm that winter apples give higher
extraction yields of pectin.
Citrus fruits are particularly rich in pectin and the large quantities
that are processed and, consequently, the considerable amounts of
wastes generated, have become the main sources for the production of
commercial citrus pectin. In citrus peel the amount of pectin has been
estimated to account for as much as 25-30% of the dry weight (Ververis
et al., 2007). The literature provides a comprehensive overview of the
pectin composition of several varieties of citrus fruits including lime,
lemon, orange, and grapefruit (Sharma, Mahato, Cho, & Lee, 2017).
Furthermore, research conducted to date has also explored the means
by which the yields and quality of pectin extracted from these sources
can be improved. Naghshineh, Olsen, and Georgiou (2013) investigated
the application of high hydrostatic pressure technology for enzymatic
extraction of pectin from lime peel and compared the extraction yields
with those obtained for acid and aqueous extraction. The latter two
extraction methods gave extraction yields of 13.4% (aqueous extrac-
tion) and 18.3% (acid extraction). Although no significant effect on
pectin characteristics was observed, pressure-induced enzymatic treat-
ment improved the pectin yield, which reached a maximum of 26.5%.
Other recent studies reported on the use of enzymatic hydrolysis and
membrane filtration for the extraction of pectin from lemon peels
(Gómez, Yáñez, Parajó, & Alonso, 2016), recovery of pectin from po-
melo peel (Methacanon, Krongsin, & Gamonpilas, 2014), and the in-
fluence of acid type and pH on the extraction of pectin from orange,
lemon, lime, and grapefruit peel (Kaya, Sousa, Crépeau, Sørensen, &
Ralet, 2014).
Another source considered for commercial pectin production was
sugar beet pulp, owing to its high pectin content (15–30%) on a dry
weight basis and its availability in large quantities due to its high
production in the sugar industry (Yapo, Robert, Etienne, Wathelet, &
Paquot, 2007). The effects of extraction parameters on the recovery of
sugar beet pectin have been extensively studied over the years. Of re-
cent studies, the work of Li et al. (2015) stands out as a comprehensive
analysis of the combined effect of pH, temperature, time, and liquid-to-
solid ratio on the extraction process. The yield of sugar beet pulp pectin
ranged from 6.3% to 23.0%; the increase in pectin yield was correlated
with increased temperature, extended extraction time, and reduced pH
of the extracting solution. By studying the emulsifying properties it was
concluded that sugar beet pectin could be used to prepare stable oil-in-
water emulsions. Even though it acts as an effective emulsifier, sugar
beet pectin applications are limited by its poor gelling properties, which
have been attributed mainly to the high acetyl content (Ralet, Crépeau,
Buchholt, & Thibault, 2003) and its greater neutral sugars content (Guo,
Guo, Yu, & Kong, 2018). However, the feruloyl groups on the arabinan
side chains of RG-I provide a way for enzyme-catalyzed oxidative cross-
linking of sugar beet pectin to promote gelation. This can be accom-
plished via horseradish peroxidase (HRP, EC 1.11.1.7) and laccase (EC
1.10.3.2) catalysis. Research conducted by Zaidel, Chronakis, and
Meyer (2012) showed that the use of laccase over HRP to catalyze
gelation has two main advantages: it produces stronger gels at lower
enzyme dosage and a slower rate of gelation, and it does not require
H2O2 for the reaction.
Besides the sources presented above, the polysaccharide content of
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Food Research International 113 (2018) 327–350
other residues of fruit and vegetable processing that are generated in
large quantities has been investigated in order to determine their
suitability as profitable sources of commercial pectin (Table 1). Special
attention was given to residues of the industrial processing of tomato
and carrot, as these are important crops in various geographical areas.
Tomato processing, mostly by the canning industry, leads to the accu-
mulation of large amounts of pomace (representing around 4% of the
fruit weight) composed of tomato peels, seeds, and a small amount of
pulp. Analysis of the composition of tomato pomace has concluded that
the by-product contains 7.55% pectin on a dry weight basis (Del Valle,
Cámara, & Torija, 2006). The possibility of utilizing tomato peel as a
cheap and abundant source for pectin production was studied by
Grassino et al. (2016) with the purpose of implementing a viable cy-
clical economy principle for solving the main problem of waste dis-
posal. Two different batches of dried tomato peel from a canning fac-
tory were used in the extraction. Based on the degree of esterification
(around 82%) the extracted pectin was categorized as HMP. Two ob-
servations made by the authors are of particular relevance for the
commercial production of pectin from tomato waste: higher pectin
yields are not necessarily correlated with higher pectin quality, and
sample origin has a considerable effect on pectin characteristics.
Similar to tomato, carrot is processed in large quantities in juice and
canning factories, and the resulting carrot pomace is usually discarded
as an industrial waste or used as animal feed. In the chemical compo-
sition of carrot pomace, pectins account for approximately 22-25% of
the total dietary fiber (29.6%) (Stabnikova, Wang, & Ivanov, 2010), a
lower content when compared to the previously presented sources of
pectin. However, the crop importance in most geographical areas and
the increased production of carrots have drawn interest in investigating
the suitability of carrot waste as a source for pectin isolation. Jafari,
Khodaiyan, Kiani, and Hosseini (2017) studied the effects of process
parameters (pH, temperature, heating time, and liquid/solid ratio) on
the extraction yield and degree of esterification of carrot pomace
pectin. Extraction yield ranged from 5.0 to 15.2% and the extracted
pectin was classified as LMP. Emulsions prepared with carrot pectin had
high stability, while 1% (w/v) carrot pectin solutions exhibited viscous
and pseudoplastic behavior. The structural characteristics of carrot
pectin were thoroughly investigated by Christiaens et al. (2015) in a
study that evaluated the extraction and properties of pectin from five
vegetable waste streams including rejected carrots and carrot steam
peels. Pectin from carrot steam peels was found to have a very high
level of linearity, a lower DM, and a better solubility than pectin ex-
tracted from rejected carrots. Because HMP and LMP are both applied
as gelling agents in the food industry, it can be concluded that both
types of carrot wastes are suitable sources for pectin production.
Watermelon rinds, which account for approximately one third of
total fruit mass and are usually discarded despite being edible (Al-Sayed
& Ahmed, 2013), were proposed as another possible source of pectin.
Regarding the pectin content, in wet watermelon rinds a level of 19-
21% (w/w) pectin was determined (Banerjee et al., 2017). Petkowicz,
Vriesmann, and Williams (2017) investigated the chemistry and rheo-
logical and emulsifying properties of pectin extracted from fresh (FW)
and lyophilized watermelon (LW) rinds in order to gain an under-
standing about its potential for use in the food industry. Fresh water-
melon rinds gave higher yields of pectin than lyophilized rinds. FW and
LW pectin had a high degree of methyl esterification (~60%) and low
molar mass. The relatively high viscosity of pectin solutions at 5% (w/
w) indicated a suitable application as thickening agents, while the good
foaming and emulsifying properties (compared to gum Arabic) sug-
gested that it can be an efficient emulsifier and stabilizing agent.
One more industrial waste introduced as source for pectin extraction
is banana peel. Since bananas are not only consumed in raw form, but
are also processed into various products, such as beverages, puree,
jellies, chips, important volumes of banana peel are discarded as waste
causing environmental problems. It was estimated that banana peels
account for about 30% of total weight of the fruit and contain a low
 F. Dranca, M. Oroian

Table 1
Physicochemical properties of pectin: main sources of commercial pectin vs. other sources.
Plant source for pectin isolation Yield of Galacaturonic acid Degree of esterification Molecular weight Neutral monosaccharide content References
pectin content
recoverya

Apple pomace Granny Smith variety 4.2% 58.6% (Granny Smith) - 52.51% (Royal variety) 331-899 kDa 14.3-31.1% Constenla et al. (2002); Kumar and Chauhan
Royal variety 16.65% 67.14% (Royal variety) - 76.4% (Granny (2010); Wikiera et al. (2016)
Golden variety 18.79% Smith)
Pomace utilized in 19.8%
commercial
production of pectin
Citrus peel Lime peel 13.4-26.3% 68.88% (mandarin 37.5% (sour orange) - 342.7 kDa (lime) - 1.33% (pomelo) - 9.3% (lime) Ara, 0.1% (lime) - Naghshineh et al. (2013); Dominiak et al.
Mandarin orange peel 21.95% orange) - 91.6% (lime) 82.2% (lime) 918 kDa (pomelo) 0.16% (pomelo) Fuc, 1.64% (pomelo) - 4.1% (lime) (2014); Methacanon et al. (2014); Wang et al.
Orange peel 24.2% Gal, 0.8% (mandarin orange) - 3.25% (pomelo) Glc, (2014); Boukroufa et al. (2015); Wang et al.
Sour orange peel 29.1% 0.62% (mandarin orange) - 1.5% (lime) Rha, 0.18% (2015); Hosseini et al. (2016); Liew et al.
Grapefruit peel 27.34% (mandarin orange) - 0.7% (lime) Xyl (2016)
Pomelo pectin 27.63-37.52%
Sugar beet pulp 23-24.87% 72.4% DM=52%, 311 kDa 24.3% Li et al. (2015); Chen et al. (2015); Guo et al.
DAc=28.1% 6.4% Ara, 13.2% Gal, 0.6% Glc, 4.4% Rha, 0.2% (2016)

332
Xyl
Tomato waste Tomato pomace 7.55% 78.4% (CBP) 76.92-88.98% n.d. 2.9% Ara, 3.85% Gal, 0.7% Glc, 3.8% Man, 1.4% Del Valle et al. (2006); Grassino et al. (2016);
Dried tomato peel 32.6% Rha, 2.3% Xyl Müller-Maatsch et al. (2016)
Carrot waste Rejected carrots 8.9% 62-69% 53-77% (WSP) 114 kDa (rejected 8-11.9% Ara, 0.12-0.18% Fuc, 13-24.4% Gal, 40.9- Christiaens et al. (2015); Jafari et al. (2017)
Carrot pomace 5-15.2% carrots) – 1460 kDa 50.6% Glc, 1.6-1.9% Man, 1.7-3.2% Rha, 0.3% Xyl
Carrot steam peels 9% (carrot steam peels) (in WSP)
Watermelon 19-21% 68.7% (LW) - 74.2% DM: 61.5% (LW) - 63% 3.451 × 104 g/mol 0.6-0.7% Ara, 0.1-0.2% Fuc, 20.2-22.6% Gal, 1.4- Banerjee et al. (2017); Petkowicz et al. (2017)
rinds (FW) (FW) (FW), 4.039 × 104 g/ 4% Glc, 0.4-0.6% Man, 2.4-2.9% Rha, 0.5% Xyl
mol (LW)
Mango peel 17.15% 29.35-53.35% DM: 85.43-88.38% 378.4-2858 kDa n.d. Wang et al. (2016)
Passion fruit 10-12.67% 66.65-68.7% DE=60.36%, n.d. n.d. Kliemann et al. (2009); Freitas de Oliveira et al.
peel DM=45.94% (2016)
Banana peel 9% 40.2-71.8% DM: 49-80%, 87-248 kDa 1-5.3% Ara, 1.6-5.7% Gal, 0.1-0.24% Rha Happi Emaga et al. (2008); Maran et al. (2017)
DAc: 1.2-5.7%
Pumpkin waste 7.4% 63.3-73.8% DM=18%, DAc=3% 139-289 kDa 4.1-4.6% Ara, 0.4-0.6% Fuc, 7.2-9% Gal, 6.6-11.2% Košťálová et al. (2016); Müller-Maatsch et al.
Glc, 0.8% Man, 4.2-4.6% Rha, 0.9-4.3% Xyl (2016)

n.d. – not determined, WSP – water soluble pectin, FW – fresh watermelon rinds, LW – lyophilized watermelon rinds, CBP - calcium-bound pectin.
a
On a dry weight basis
Food Research International 113 (2018) 327–350
F. Dranca, M. Oroian
amount of water-soluble pectin (Happi Emaga, Ronkart, Robert,
Wathelet, & Paquot, 2008). Maran et al. (2017) reported on the opti-
mization of the process parameters in pectin extraction from industrial
banana waste. At optimum levels of extraction parameters, the yield of
pectin was approximately 9% (w/w). More research is needed re-
garding the chemistry and especially the properties of pectin from ba-
nana peel prior to establishing whether or not this has potential in the
food industry as a gelling, thickening, or stabilizing agent.
The previously outlined findings show that most of the research
conducted to date is focused on singular fruit and vegetable residues as
sources of commercial pectin, an understanding that is actually vali-
dated by the literature. Of the few studies that investigate several
sources of pectin and have been published up to this point, unarguably
the most complete survey of pectic materials obtained from many di-
verse by-products belongs to Müller-Maatsch et al. (2016). The re-
searchers selected 26 food waste streams according to their exploitation
potential, isolated the contained pectin and fully characterized it in
terms of uronic acid and other sugar composition, methylation, and
acetylation degrees. The structure of pectin extracted from these waste
streams seemed generally well preserved when compared to the ori-
ginal food material; notable exception to this observation were the
methylation and acetylation degrees that were often lowered either by
processing and/or enzymatic action. Finally, although the minimum
requirement of 65% uronic acids prevented some of the plant residues
to the considered sources for pectin extraction, it was noted that these
waste streams could be useful in other applications.
Important properties such as galacturonic acid content, degree of
esterification, molecular weight, neutral monosaccharides content of
samples isolated from main sources of commercial pectin and other
vegetal sources are presented in Table 1. Among citrus pectin sources,
pomelo has shown a galacturonic acid content and degree of ester-
ification (Methacanon et al., 2014) greater than other wastes commonly
used in pectin extraction (e.g. orange peel). Properties which influence
the use as a gelling agent, thickening agent and stabilizer, and which
show promising applications, can be also noted for pectin from tomato
waste, pumpkin waste, and watermelon rinds.
Any approach to selecting suitable pectin sources should take into
account that pectin structure and yield are highly diverse according to
origin. Furthermore, for the same waste stream possible variations in
pectin characteristics and content may be due to differences between
batches and countries. However, the information presented here offers
a good insight into pectin composition and its modification after pro-
cessing, both of which are valuable for the industry when introducing
new sources of commercial pectin. The possible uses of pectic poly-
saccharides, which derive from the data obtained in the previously
described studies, are also greatly influenced by the choice of extraction
technique and the purification method.
4. Extraction, purification and fractionation
The entire production process of pectin has been completely docu-
mented in the literature and generally is comprised of three stages: a
pretreatment, the extraction operation, and a post-extraction stage. The
purpose of the pretreatment, whether a drying, washing, or blanching
process, is to increase the stability of the raw material by inactivating
bacteria and enzymes that otherwise cause pectin degradation. On the
industrial scale, the second stage of pectin production is the extraction,
which combines the presence of a mineral acid (such as hydrochloric
acid, sulfuric acid, or nitric acid) with a heat treatment. The use of this
conventional acid extraction method raises some questions regarding
resource management. Because the prolonged length of the process, and
especially the heating, is linked to increased energy consumption, it is
important to determine if the economic demands are justified by the
production of high-quality pectin or if it is possible to reduce the overall
cost of the process without affecting the quality of the pectin. The same
principle should be also considered in the context of an efficiency
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Food Research International 113 (2018) 327–350
evaluation for alternative extraction techniques.
4.1. Extraction techniques
Pectin extraction is defined as a physical-chemical process which is
comprised of multiple stages of hydrolysis and extraction of pectin
macromolecules from plant tissue and their solubilization into the bulk
solvent, all of them occurring in a continuous manner under the in-
fluence of different process parameters, mainly temperature, pH, and
time (Methacanon et al., 2014). Pectin is a complex macromolecule,
and the preservation of its structure, which determines characteristics
such as molecular weight, water solubility, and gelation properties, is
connected to the extraction method applied in its isolation from the
plant material. The extraction and isolation of pectin from cell walls can
be approached in various ways through the use of chemical, physical, as
well as enzymatic treatments (Panouillé, Thibault, & Bonnin, 2006).
Among the chemical methods, acid extraction seems to be the most
widely used in commercial pectin production.
4.1.1. Solvent extraction
The use of a suitable method, alongside a good understanding of the
individual and collective effect of process parameters is essential in
order to maximize pectin yield and its quality. In the particular case of
solvent extraction, the type of extraction solvent, its concentration, and
operation conditions such as pH, temperature, and extraction time
impact the release of pectin from the cell wall. The study of the para-
meters involved in solvent extraction is not a novelty subject in the
literature, as it has been widely studied through the years.
In regard to extraction solvent, an ideal choice should feature the
following desirable characteristics: the solvent has a high capacity for
the solute separated into it, it is selective, can dissolve the specific
component to a large extent while having a minimum capacity for other
components, is chemically stable, renewable, and has a low viscosity,
which eases pumping and transportation (Oroian & Escriche, 2015).
Accordingly, when studying the extraction efficiency of a solvent, not
only the pectin yields are of relevance, but also its structure and che-
mical composition because these are known to govern its applications.
Commonly used solvents are diluted strong mineral acids. Kalapathy
and Proctor (2001) investigated the effect of hydrochloric acid strength
(0.05, 0.1, 0.2, and 0.3 N) on the yield and purity of pectin extracted
from soy hull. It was reported that the highest yields (26 and 28%) were
obtained when the acid strength was 0.05 and 0.1 N, and that a further
increase in acid strength caused a decrease of pectin yield. Unlike the
strong effect on extraction yield, strength of acid did not affect pectin
purity. Besides solvent strength, the influence of solvent type on pectin
extraction was also studied. Begum, Aziz, Uddin, and Yusof (2014)
carried out a comparison of extraction solvents (ammonium oxalate,
diluted sulfuric acid, and sodium hexametaphosphate) for the isolation
of pectic substances from jackfruit. It was found that acid extraction
gave the lowest extraction yield (8.94%); in contrast, extraction with
sodium hexametaphosphate gave the highest yield (15.14%), but the
isolated pectin had high ash content and the lowest solubility. Com-
parison between extraction solvents was extended to analyzing the ef-
ficiency of mineral acid extraction against the extraction of pectin with
organic acids. Kliemann et al. (2009) investigated the extractability of
pectin from passion fruit waste using three kinds of acid, citric, hy-
drochloric, and nitric acids. The best extraction yield was obtained with
citric acid, and the extracted pectin was rich in anhydrogalacturonic
acid and had a low DM. The high efficiency of citric acid in pectin
extraction was also confirmed by Chan and Choo (2013) when com-
pared to the pectin yields determined for hydrochloric acid, and by
Yang, Mu, and Ma (2018) following an investigation on the effects of
the extraction of potato pectins with hydrochloric, sulfuric, nitric, ci-
tric, and acetic acids. These differences in yield and pectin quality be-
tween acids can be explained by 2 separate phenomena: (a) when
combined to increased temperatures and prolonged extraction time,
F. Dranca, M. Oroian
strong acid solutions (e.g. hydrochloric acid) could enhance pectin
hydrolysis and hence result in a more degraded, shorter pectin chain;
(b) the additional extraction activity of citric acid on chelator-solubi-
lised pectin fraction leads to increased yields when compared to mi-
neral acids, under identical extraction conditions (Jamsazzadeh
Kermani et al., 2014; Maneerat, Tangsuphoom, & Nitithamyong, 2017).
Considering that strong mineral acids are corrosive, are deemed a po-
tential threat to health, and are linked to possible increased costs of
waste treatment, the extraction using citric acid and other weak organic
acids may bring a major advantage to the overall process of pectin
isolation.
Pectin extraction from fruit and vegetable residues using weak or-
ganic acids has been intensively studied, suggesting that numerous data
regarding the influence of operating conditions on pectin yield and
quality is available. Alba, Laws, and Kontogiorgos (2015) designed an
isolation protocol to extract pectin from okra with citric acid and stu-
died the influence of the extraction pH (6.0 or 2.0) on the composition
and physicochemical properties of the polysaccharides. Extraction with
citric acid adjusted to pH 6.0 resulted in higher pectin yield compared
to that at pH 2.0. The extraction conditions determined some structural
variations between samples: pectin polysaccharides extracted at pH 2.0
had a lower content of neutral sugars and galacturonic acid, while
pectin obtained by extraction at pH 6.0 had lower DM and DAc. In-
fluence of pH (2.0, 3.3, or 4.5), alongside that of the extraction time
(30, 75, or 120 min) on pectin yield and composition was also studied
by Liew, Chin, and Yusof (2014) in a citric acid extraction process. The
maximum extraction yield was found at 75 min and the lowest pH; of
these two factors, pH showed a greater influence on pectin yield. On the
other hand, the degree of esterification was significantly affected by
extraction time. A more complete analysis of the involved factors was
conducted by Pereira et al. (2016) who evaluated the influence of pH
(2–4), temperature (70–90 °C), and time (40–150 min) on pectin ex-
traction from pomegranate peels with citric acid. Based on the results, it
was noted that harsh extraction conditions (low pH, high temperatures,
and prolonged extraction) determined higher pectin yields and higher
galacturonic acid contents, while causing a decrease in the degree of
methylation. This conclusion regarding the combined positive impact of
low pH values, high temperature and prolonged extraction time on the
extraction yield of pectin is corroborated in numerous studies, as it can
be deduced from the data presented in Table 2. Alongside studying the
influence of operating conditions on pectin yield and quality, the var-
ious factors affecting pectin extraction from plant sources, including
extraction temperature, pH, time, and liquid/solid ratio (LSR) are op-
timized in order to achieve a maximum yield and the desired char-
acteristics of pectin. Numerous studies were aimed to optimize the
process variables in the extraction of pectin from wastes such as sour
orange peel (Hosseini, Khodaiyan, & Yarmand, 2016), durian rinds
(Maran, 2015), lime peel (Andersen et al., 2017), and Valencia orange
peels (Casas-Orozco, Villa, Bustamante, & González, 2015), for the
latter two plant sources the process being designed for an industrial-
scale extraction. Important findings of research on pectin extraction
conducted with different solvents in specific conditions are summarized
in Table 2.
4.1.2. Novel extraction techniques
The development of green chemistry has impacted the isolation step
of the analysis of macromolecules from plants and, as a result, in the
last few years environment-friendly techniques have emerged as an
alternative to the traditional acid extraction method. Current research
aims at optimizing cleaner extraction techniques such as enzyme-as-
sisted extraction, microwave-assisted extraction, ultrasound-assisted
extraction, subcritical water extraction, and induced electric field ex-
traction. The first four techniques have been recently reviewed in pectin
production by Adetunji, Adekunle, Orsat, and Raghavan (2017), who
covered all the particularities from principles and operational issues to
benefits and drawbacks. Important results regarding the application of
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Food Research International 113 (2018) 327–350
these techniques in pectin isolation and the influence of extraction
parameters are presented in Table 2. The conditions of enzyme-assisted
extraction were studied in several researches including the works of
Dominiak et al. (2014), Jeong et al. (2014), Wikiera, Mika, and
Grabacka (2015), Wikiera, Mika, Starzyńska-Janiszewska, and Stodolak
(2015), and Wikiera, Mika, Starzyńska-Janiszewska, and Stodolak
(2016), some of them being summarized in Table 2. The potential of
ultrasound-assisted extraction (UAE) of pectin was studied for plant
sources such as from passion fruit peel (Freitas de Oliveira et al., 2016),
grapefruit peel (Wang et al., 2015; Xu et al., 2014), mango peel (Wang
et al. (2016), and jackfruit peel (Moorthy et al., 2017). It should be
mentioned here that when studying the simultaneous effect of tem-
perature and ultrasound treatment it is crucial to consider that ultra-
sounds cause a disintegration of the material, consequently affecting
the separation of solid and liquid phases. This may translate into a
lower pectin yield of the ultrasound-assisted heating extraction by
comparison with a conventional heating process. To avoid erroneous
conclusions regarding the effect of temperature and sonication on ex-
traction yields, a second UAE is recommended in order to completely
dissolve the pectin previously absorbed in the residue.
As in the case of the previous extraction techniques, that are pre-
sented in Table 2, microwave-assisted extraction (MAE) has been ap-
plied to extract pectin from wastes of fruit and vegetable processing,
including unutilized pumpkin biomass (Košťálová, Aguedo, &
Hromádková, 2016), the waste peels of papaya (Maran & Prakash,
2015) and mango (Maran, Swathi, Jeevitha, Jayalakshmi, & Ashvini,
2015), tangerine peels (Chen et al., 2016), and Opuntia ficus indica
cladodes (Lefsih et al., 2017). Along the years the work of Fishman and
collaborators on the extraction of pectin from orange albedo (Fishman,
Chau, Hoagland, & Ayyad, 1999), lime (Fishman, Chau, Hoagland, &
Hotchkiss, 2006), and sugar beet pulp (Fishman, Chau, Qi, Hotchkiss, &
Yadav, 2013) brought notable contribution to the knowledge regarding
the use of microwaves in the extraction of pectin from plant materials.
Some research has been conducted in the last years with the purpose of
studying the use of microwave-assisted extraction and ultrasound-as-
sisted extraction as complementary techniques for the isolation of
pectin from vegetable sources. Bagherian, Zokaee Ashtiani,
Fouladitajar, and Mohtashamy (2011) described the results of a MAE of
pectin from grapefruit peel where a preliminary ultrasonic heating of
grapefruit solution was introduced. They observed that this pretreat-
ment provided a higher pectin yield, especially in the case of inter-
mittent sonication. Regarding the composition of pectin extracted
through a sequential ultrasound-microwave-assisted extraction, Liew,
Ngoh, Yusoff, and Teoh (2016) reported that the combined extraction
technique resulted in a higher GalA content because it allows a more
complete release of the pectin compound and therefore a better pre-
servation of the GalA distribution from deeper plant matrix than a sole
ultrasound or microwave extraction. The combination of microwave
and ultrasound treatment alongside the use of “in situ” water, which
was recycled and used as solvent, allowed Boukroufa, Boutekedjiret,
Petigny, Rakotomanomana, and Chemat (2015) to obtain valuable
compounds (pectin, essential oil, and polyphenols) from orange peels
waste in a shorter time. Citrus waste, such as flavedo of Citrus junos
(Ueno, Tanaka, Hosino, Sasaki, & Goto, 2008), Citrus junos peel
(Tanaka, Takamizu, Hoshino, Sasaki, & Goto, 2012), and citrus peel
(Wang, Chen, & Lü, 2014), was also used as a source for the subcritical
water extraction of pectin; the same extraction technique was applied
for the isolation of pectin from apple pomace (Wang et al., 2014) and
sugar beet pulp (Chen, Fu, & Luo, 2015), as shown in Table 2.
Another novel technique applied for the isolation of pectin from
plant materials is induced electric field-assisted extraction. Application
of induced electric field for the extraction of targeted compounds is
based on the use of inductive methodology, which represents an al-
ternating magnetic flux creating an alternating voltage in accordance to
Faraday’s law of induction. The induced electric field acts upon the
biological tissue and, as a result, different phenomena, including
 Table 2
Extraction techniques and their effects on pectin yield and quality.
Extraction technique Plant source Operating conditions Effect on yield and quality References

Solvent extraction Cocoa husks Solvent: water, citric acid or hydrochloric acid The highest pectin yield (7.62%) was obtained Chan and Choo (2013)
F. Dranca, M. Oroian

Enzyme-assisted extraction
pH: 2.5 or 4.0 using citric acid (pH 2.5, 95°C, 3.0 h), while the
Temperature: 50 or 95°C highest uronic acid content in pectin (65.20%)
Time: 1.5 or 3.0 h resulted by using water (95°C, 3.0 h).
Extraction with citric acid produced pectin with a
wider DM range.
Sour orange peel Solvent: water The yield of pectin extracted at the optimal Hosseini et al. (2016)
Liquid/solid ratio: 20:1, 30:1 or 40:1 (v/w) condition (95°C, 90 min, and liquid/solid ratio of
Temperature: 75, 85 or 95°C 25:1) was 18.35%. GalA content and DE of the
Time: 30, 60 or 90 min extracted pectin ranged from 57% to 83%, and 17-
30.5%, respectively.
Durian rinds Solvent: water Under optimal conditions (solid/liquid ratio of Maran (2015)
Solid/liquid ratio: 1:5-1:15 (g/mL) 1:10 g/mL, pH of 2.8, 43 min, 86°C) the pectin
pH: 2-3 yield reached 9.1%.
Temperature: 75-95°C
Time: 20-60 min
Lime peel Solvent: water:nitric acid Higher pectin solution concentrations were Andersen et al. (2017)
pH: 1.5, 2.3 or 3.1 obtained at the lower pH values. Increased
Temperature: 60, 70 or 80°C temperature and especially acidity caused a faster
decrease of DE, effect that was particularly
significant during extractions at pH=1.5.
Apple pomace Enzymes: xylanasea and multicatalytic Polygalacturonic acid was completely hydrolyzed Wikiera et al. (2015)
preparation Celluclast after 2.5 h incubation with 2 M TFA at 120°C.
Acid used in extraction: trifluoroacetic acid 2M Prolonged extraction was positively correlated
Temperature: 100 or 120°C with an increase of GalA released.

335
Time: 1, 1.5, 2, 2.5, 3 or 4 h Efficient release of neutral sugars was performed at
100°C for 2.5 h.
Apple pomace Enzymes: endo-xylanase and endo-cellulaseb Treatment with endo-xylanase resulted in the Wikiera et al. (2016)
Solid/liquid ratio: 1 g/15 mL highest pectin yield (19.8%) and very high DM
Enzyme dose: 50 U/g (73.4%). Pectin extracted by endo-cellulase
pH: 5.0 treatment was characterized by the high GalA
Temperature: 40°C content (70.5%).
Time: 10 h Simultaneous use of both enzymatic preparations
resulted in a 10.2% extraction yield, and a pectin
rich in galacturonic acid (74.7%).
Rapeseed cake Commercial enzymes: Celluclast and Alcalase The optimized conditions for an improved pectin Jeong et al. (2014)
Enzyme/rapeseed cake ratio: 1:50 to 1:65 (v/ yield (6.85%) without significant loss of GalA were
w) a 1:50 enzyme/RSC ration with a Celluclast/
Celluclast/Alcalase ratio: 0:5, 1:4, 2:3, 3:2, 4:1 Alcalase ratio of 1:4 for a 270 min hydrolysis time.
or 5:0 (v/v) Enzymes indicated different functions: Alcalase led
Time: 90, 180, 270, 360 or 450 min to the destruction of protein-carbohydrate
complexes, while Celluclast slightly cleaved some
linkages of carbohydrate.
Lime peel Enzymes: Laminex C2K, Multifect B, GC220, Laminex C2K preparation proved to the most Dominiak et al. (2014)
and effective, as in optimum conditions (4 h treatment
GC880 at pH 3.5, 50°C) gave a high yield (23%) and a
pH: 3.5-6.5 pectin with good composition and properties
Temperature: 40-70°C (gelling, stabilization).
Ultrasound-assisted extraction Passion fruit peel Extraction solvent: 1.0 mol/L HNO3, pH 2.0, The highest pectin yield (12.67%) was obtained at Freitas de Oliveira et al.
peel/solvent ratio of 1:30 (g/mL) 85°C and a power intensity of 664 W/cm2. Despite (2016)
Temperature: 45-85°C the fact that pectin isolation reached the highest
Power intensity: 132.8-664.0 W/cm2 level, the isolate did not displayed the best
Time and frequency (constant): 10 min, 20 kHz composition, as the GalA content and DE showed
minimum values.
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Food Research International 113 (2018) 327–350
 Table 2 (continued)

Extraction technique Plant source Operating conditions Effect on yield and quality References

Mango peel Extraction solvent: citric acid, pH 2.5, peel/ Extraction yield of pectins varied greatly with the Wang et al. (2016)
solvent ratio of 1:40 (g/mL) increase in temperature, from 2.09% (at 20°C) to
F. Dranca, M. Oroian

Microwave-assisted extraction
Time and frequency (constant): 15 min, 20 kHz
Temperature: 20 or 85°C
Jack fruit peel Extraction solvent: distilled water)
Liquid-solid ratio: 10:1-20:1 (mL/g)
pH: 1-2
Sonication time: 15-30 min
Extraction temperature: 50-70°C
Grapefruit peel Emitter surface: 13 mm or 25 mm
Power density: 0.20, 0.27, 0.33, 0.40, 0.47 or
0.53 W/mL
Duty cycle: 33%, 40%, 50%, 60%, 70% or 80%
Temperature: 30, 40, 50, 60, 70 or 80°C
Solid-liquid ratio: 1/30, 1/40, 1/50, 1/60 or 1/
70 (g/mL)
Sonication time: 10, 20, 30, 40, 50 or 60 min
Waste papaya peel Microwave power: 320, 480 or 640 W
pH: 1, 2 or 3
Time: 20, 100 or 180 s
Solid-liquid ratio: 1:5, 1:15 or 1:25 g/mL
Waste mango peel Microwave power: 160, 320 or 480 W
17.15% (at 85°C). A significant influence of
temperature was also observed for GalA content
(increase from 29.35% to 53.35%) and molecular
weight (increase from (378.4 kDa to 2320 kDa).
Optimal conditions for the extraction were: liquid- Moorthy et al. (2017)
solid ratio of 15:1 mL/g, pH of 1.6, sonication time
of 24 min, and temperature of 60°C. Under this
conditions the pectin yield was 14.5%
Heating significantly improved the extractability Xu et al. (2014)
and extraction rate of pectin, leading to higher
yield (26.74%) in shorter extraction time (51.79
min).
The optimized parameters were: ultrasound power
density 0.40 W/mL, duty cycle 50%, temperature
60°C, S/L 1/50 g/mL.
All the process variables had significant effect on Maran and Prakash
pectin yield. (2015)
The optimal conditions for reaching a maximum
pectin yield (25.41%) were: microwave power of
512 W, pH of 1.8, time of 140 s and solid-liquid
ratio of 1:15 g/mL.
For all process parameters a similar influence was Maran et al. (2015)

336
pH: 2, 3 or 4 observed: the increase in their level was positively
Time: 60, 120 or 180 s correlated with the pectin yield up to a certain
Solid-liquid ratio: 1:10, 1:20 or 1:30 g/mL point, beyond which their effect on pectin
extraction was negative.
The maximum pectin yield (28.86%) could be
obtained at a microwave power of 413 W, pH of
2.7, time of 134 s and solid-liquid ratio of 1:18 g/
mL.
Tangerine peels Microwave power: 600, 700 or 800 W The optimal extraction parameters were: Chen et al. (2016)
Temperature: 40, 50 or 60°C microwave power 704 W, 52.2°C extraction
Time: 30, 40 or 50 s temperature, and extraction time of 41.8 min.
Under these conditions the experimental yield of
pectin was 19.9 ± 0.2%.
Opuntia ficus indica Microwave power: 200, 400 or 600 W The optimum conditions to obtain a maximum Lefsih et al. (2017)
cladodes pH: 1.5, 2.25 or 3 pectin recovery of 12.56% were 2.16 min, pH 2.26,
Time: 1, 2 or 3 min 517 W microwave power and 2 g/30.66 mL of
Solid-liquid ratio: 2:20, 2:35 or 2:50 g/mL solid-liquid ratio.
FTIR analysis indicated a GalA content of 34.4%
and no alterations in the chemical structure of
pectin following microwave treatment.
Subcritical water extraction Apple pomace and Solid to liquid ratio of 1:30 g/mL, extraction The highest yield (21.95%) of citrus pectin Wang et al. (2014)
citrus peel time of 5 min (constant) (68.88% GalA content) was obtained at 120°C, and
Extraction temperature: 130°C, 150°C or 170°C the highest yield of apple pectin (16.68%) was
C for apple pomace; 100°C, 120°C or 140°C for gained at 150°C (GalA content of 40.13%).
citrus peel Differential scanning calorimetry analysis showed
that the endothermic property of pectin was
affected by extraction temperature while the
exothermic property was only affected by its
constituents and raw material.
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F. Dranca, M. Oroian Food Research International 113 (2018) 327–350

intracellular liquid release and diffusion of solutes, develop inside the

cellular structure following the treatment (Vorobiev & Lebovka, 2009).
Chen et al. (2015)

Yang et al. (2016)

Therefore, utilization of an electrical driving force as auxiliary energy
leads to substantial improvements of mass transfer and extraction ef-
References

ficiency (Yamini, Seidi, & Rezazadeh, 2014). Yang, Jin, Tian, Jin, and
Xu (2016) developed an experimental system to extract pectin from
orange peel waste that, unlike other electric field-assisted techniques,
avoids the use of powered electrodes. The experimental system contains
a power source, circulating water bath, a ferrite o-core, primary coil,
glass spiral (supporting the tube of the secondary coil), glass chamber,
sample, and solution inlet, and also a sand filter. In the process the
up to a certain level past which a decrease of pectin

maximum yield of 24.63% (with 59.12% GalA and

on the extraction. Lower pH also provided a higher

Increase in all parameters enhanced the extraction

The electrical effect was found to predominate at

temperatures below 45°C, and the joint electrical
increase in frequency that had a negative impact
ratio of 44.03, 120.72°C extraction temperature,
21.66% arabinose content) were as follows: L/S

extractant (dilute hydrochloric acid) acts as a secondary coil connected

The optimum extraction conditions to obtain a

and thermal effects governed the extraction at

enhancement of pectin yield, opposite to the
extraction time of 30.49 min and extraction

to the glass chamber which forms a closed loop. Through this setup the
induced electric field in the system appears to be under the influence of
An increase in excitation voltage caused

alternating magnetic flux. Table 2 presents data regarding the in-

vestigated effect of excitation voltage, frequency, temperature, and pH
temperatures from 45 to 65°C.
on pectin yield.
Effect on yield and quality

recovery was recorded.

pressure of 10.70 MPa.

4.2. Purification and fractionation of pectin polysaccharides

In early approaches to the study of pectin it was considered that the

pectin yield.

presence of adventitious substances (such as sugars and acids) must be

excluded as far as possible and a definition of what constitutes “pure”
pectin was necessary. In this context, the following methods of pectin
purification were acknowledged: precipitation, dialysis, ionic exchange,
nitration, as well as combined methods (Lampitt, Money, Judge, & Urie,
1947). Precipitation is a method generally employed to purify the
pectin contained in an aqueous extract through subsequent washings
with alcohol or acetone. Alcohol precipitation is frequently used at both
laboratory and industrial scales because it gives satisfactory pectin
Liquid/solid ratio: 30, 40 or 50 (w/w)

yields at advantageous costs. Guo et al. (2016) proved that a stepwise

Extraction pressure: 8, 10 or 12 MPa
Temperature: 110°C, 120°C or 130°C

ethanolic precipitation is a more effective method for the purification of

Extraction time: 20, 30 or 40 min

sugar beet pectin (SBP) than a one-step ethanolic precipitation. They

Solvent: diluted hydrochloric

Excitation voltage: 0-300 V

also noted that the ethanol concentration required for purification was
dependent on pectin structure, and particularly the proportion of neu-
Frequency: 20-200 kHz
Temperature: 20-80°C
Operating conditions

tral side chains. Based on their results, the researchers indicated that at
least a concentration of 75% ethanol is recommended to obtain a sa-
pH: 2, 3 or 6.8

tisfactory yield of purified sugar beet pectin. However, the purity of

pectin obtained only through alcoholic precipitation was found to be
lower when compared to the composition of pectin purified by ultra-
Acid

filtration and metal ion-binding precipitation. Yapo, Wathelet, and

Paquot (2007) compared alcoholic precipitation to the purification of
pectin by ultrafiltration-diafiltration (Table 3) and reported that the use
of the first technique resulted in more neutral sugars, more proteins,
and more ash, but less galacturonic acids in sugar beet pectin. In con-
trast, ultrafiltration has been reported to effectively remove impurities
Orange peel waste
Sugar beet pulp

such as pigments and salts (Kang, Hua, Yang, Chen, & Yang, 2015),
Plant source

while metal ion-binding precipitation proved to be selective toward

binding HG and RG regions and thereby is suitable to purify pectins
from non-uronide contaminants (Guo, Meng, Zhu, Zhang, & Yu, 2015).
Although it presents a great advantage of a better selectivity towards
adventitious compounds, metal ion-binding precipitation is likely to
generate, at an industrial scale, a large amount of effluents that demand
treatment prior to their discharge in order to avoid environmental da-
mage. By considering this main drawback, Yapo (2009) concluded that
Induced electric field-assisted extraction

it would be more advantageous to precede alcohol precipitation with an

industrially-practical membrane procedure (such as ultrafiltration-dia-
filtration) for an effective removal of pectin contaminants that assures
the compositional quality and gelling properties of the final pectin
product.
Extraction technique
Table 2 (continued)

Apart from the techniques presented above (Table 3), the literature
EC 3.2.1.8.

provides other new methods that have been developed with the purpose
EC 3.2.1.4

of achieving a better purification of pectin. Garna, Emaga, Robert, and

Paquot (2011) proposed a technique for the purification of electrically
charged polysaccharides using protein (sodium caseinate). The pur-
b
a

ification is based on the electrostatic interactions taking place between

337
F. Dranca, M. Oroian
Table 3
Methods of pectin purification: comparative view and new approaches.
Method Procedure
Alcohol precipitation with A first washing of crude pectin with 60% (twice), 70%
washing (twice) and 80% ethanol, followed by a final washing step
with 96% ethanol (twice). The final gel was recovered in
water, freeze-dried, vacuum-dried at 40°C.
Stepwise ethanol- Precipitation with an equal volume of ethanol in elevated
precipitation concentration from 50% to 80% (v/v) followed by
centrifugation, ethanol washing and lyophilization.
Ultrafiltration in Purification was performed using hollow fiber tangential
combination with flow filtration membranes (polysulfone, 0.5 mm i.d, 615
diafiltration cm2) of 10 and 50 kD MWCOs.
Ultrafiltration The ultrafiltration was conducted under 15 bar at 40°C using
a membrane with a surface area of 1.77 m2 and a molecular
weight cut-off of 8000 Da.
Metal precipitation Precipitation of the extract with a solution of CuSO4∙5H2O
followed by centrifugation, filtration and washing with HCl
and ethanol to eliminate Cu2+ ions.
Copper precipitation Precipitation of pectin with aqueous CuSO4 completed with a
dispersion of EDTA solution in the filtration cloth for the
extraction of copper ions from the copper-pectin complexes.
Purification using protein Precipitation takes place after the addition of caseinate (pH
(sodium caseinate) 3.5; 10 g/l); to separate pectins from sodium caseinate the
pH is increased to 6.5 by adding 1M NaOH, NaCl is added
after the dissolution of the pellet, followed by 0.1M HCl to
decrease pH to 4.6 (precipitation of caseinate).
the two polymers and is comprised of two steps: a first step where the
charged pectins are precipitated using proteins at pH 3.5, and a second
step in which the polymers are separated by the dissociation of the
pectin-caseinate complexes and the precipitation of caseinate at a pH
close to its isoelectric point (pH 4.6). The feasibility of the process was
verified through application on commercial pectin from apple pomace,
and the results indicated that this purification method is very effective
for the recovery of charged polysaccharides. Happi Emaga, Garna,
Paquot, and Deleu (2012) then applied this technique to purify apple
pomace pectin and evaluated its efficiency against purification by
ethanol precipitation. It was observed that, under certain conditions,
ethanol caused the precipitation of other compounds, but allowed total
precipitation of pectin when compared to caseinate. The use of case-
inate has the advantage of a higher specificity for the charged polymer,
which is substantially overshadowed by the drawback of requiring a
large quantity of protein.
When the objective of the research is to fully elucidate the com-
position of the extracted pectin, purification is usually performed to-
gether with a fractionation which can be achieved through various
techniques. For example, Lin et al. (2016) fractionated the crude
polysaccharide obtained from flowers of Lonicera japonica by anion-
exchange chromatography performed on a DEAE-cellulose52 column,
where a stepwise elution with water gave six different fractions; the
major fraction (LJ-02) was further purified with a Sephacryl S-200HR
column. Fractionation allowed the evaluation of antipancreatic cancer
activity, which concluded in the finding that a RG-I polysaccharide
from Lonicera japonica flowers could be a potential novel therapeutic
agent against pancreatic cancer. To elucidate the structure of an im-
mune-enhancing pectic polysaccharide from the aqueous extract of
green bean pods, Patra, Das, Behera, Maiti, and Islam (2012) subjected
the crude polysaccharide to purification and fractionation by gel per-
meation chromatography on a column of Sepharose 6B and water as an
eluant using a fraction collector. The isolated water-soluble pectin
contained a [→4)-α-D-GalpA6Me-(1→4)-α-D-GalpA6Me-(1→] back-
bone with branching at C-2 and showed significant antioxidant activity
and thymocyte and splenocyte activation. The beneficial effects of se-
parate structures from the composition of pectin polysaccharides was
also investigated by Li, Xia, Nie, and Shan (2016) who fractionated the
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Food Research International 113 (2018) 327–350
Effect on extract References
The technique gave a higher pectin yield, and the isolate Yapo, Wathelet, and
contained more neutral sugars, proteins, and ash but had a Paquot (2007)
galacturonic acid content lower than a pectin sample
purified by ultrafiltration.
Pectin fractions rich in neutral sugars were precipitated at Guo et al. (2016)
relatively high ethanol concentrations.
The stepwise precipitation is more selective with respect to
pectin structural features and surface properties than a one-
step process.
Pectin isolated from the crude aqueous extract by the 10kD Yapo, Wathelet, and
membrane procedure contained more GalA and less neutral Paquot (2007)
sugars, suggesting a higher purity of the pectin extract.
Most of the salts and pigments were removed from the Kang et al. (2015)
sample which also had a low protein and acid-insoluble ash
content.
Pectin purified through this method had a higher Yapo (2009)
galacturonic acid content and a low neutral sugars, protein
and ash content.
Significantly higher yield and GalA content and lower Guo et al. (2015)
neutral sugar and protein content by comparison to the un-
precipitated sample.
Whatever the precipitation conditions, the purity of extracts, Happi Emaga et al.
expressed as GalA content, was lower in pectin purified by (2012)
caseinate than in that purified by ethanol (96%)
precipitation. However, pectins purified by caseinates are
characterized by a lower total content of neutral sugars.
hydrolysate from orange peel via membrane separation into three dif-
ferent molecular weight fractions that had prebiotic and antimicrobial
properties. When the three fractions were compared, it was noted that
one of them had glucose as the main component, presented higher
galacturonic acid content, and also contained high amounts of arabi-
nose and galactose, which ranked third and fourth among components.
Membrane separation, more exactly ultrafiltration, was also employed
in the fractionation of crude extract from star fruit, which led to elu-
cidating the structure of pectic type II arabinogalactans from its com-
position (Leivas, Iacomini, & Cordeiro, 2016).
Adopting the high-throughput and fractionation techniques used by
Nguema-Ona et al. (2012) to profile the different wall polymers present
in the leaves of Nicotiana tabacum, Moore et al. (2014) reported on the
profile of main cell wall polysaccharides of grapevine leaves. In both
studies the alcohol-insoluble residue was chemically and enzymatically
fractionated. The enzymatic fractionation procedure was performed
with glycosyl hydrolases (endopolygalacturonase, EC 3.2.1.15) and two
different xyloglucan-specific endoglucanases (EC 3.2.1.151). The two
procedures caused a sequential degradation of the recovered residue
which ended in the structural reveal of the major sub-networks, pectin
and hemicellulose, from grapevine leaves.
5. Characterization of pectin composition and properties
The analysis of pectic carbohydrates isolated from the cell walls of
various plants presents a major challenge because of the variation and
the complexity of non-uronide compounds associated with these car-
bohydrates. Similar to most other polysaccharides, pectin is poly-
molecular and polydisperse, meaning it is heterogeneous in both che-
mical structure and molecular weight (BeMiller, 1986). In regards to
chemical structure, galacturonic acid and neutral sugars are the major
constituents of pectin chains. The number and percentage of individual
monomeric units varies from molecule to molecule in any pectin
sample, while the distribution of molecular weights is determined by
source and the conditions of isolation and other treatments applied
following the recovery of pectin polysaccharides. The variability in the
structure of pectin chains, including the number of esterified methoxyl
groups to galacturonic acid, the differences in molecular weight, and
F. Dranca, M. Oroian Food Research International 113 (2018) 327–350

Table 4
Analytical methods for pectin characterization.
Parameter Analytical method References

Monosaccharide Hydrolysis, derivatization (alditol acetates) and quantification by GC and mass
composition spectrometric detection
TFA hydrolysis, HPAEC-PAD assay
Galacturonic acid content Hydrolysis, carbazole-H2SO4 reaction and spectrophotometric detection
Hydrolysis, m-hydroxydiphenyl sulfuric acid assay and spectrophotometric
detection
Combined TFA-enzymatic hydrolysis, HPAEC-PAD assay;
TFA hydrolysis and analysis by HPAEC-FID
Glycosidic linkage Methylation-induced cleavage of the glycosidic linkages, conversion to PMAAs,
conformation GC-MS assay
Methylation, identification of glycosidic linkage and side chain location by 1D
and 2D NMR
Degree of substitution Hydrolysis and acidification of pectin, headspace solid-phase microextraction
(Carboxen-PDMS fiber assembly), separation of methanol and acetic acid by
GC and detection using electron impact MS with selected ion monitoring
Hydrolysis of pectin in NaOH/D2O, direct 1H NMR analysis
Simultaneous determination of methylation and acetylation degree of pectin by
FT-IR;
Analysis of the degree of methyl-esterification by FT-IR with peak
deconvolution for protein-rich samples
Determination of methylation and acetylation degree by FT-Raman
Detection using a μSI-LOV system (includes a VIS–NIR-diode array
spectrophotometer) with ultra-pure deionized water as carrier
Degree of blockiness Pectin digestion, separation and quantification using HPAEC-PAD at pH 5
Determination by capillary electrophoresis using phosphate as buffer in an
automatic system equipped with a UV detector
Molecular weight High performance size exclusion chromatography with refractive index
detector (HPSEC-RID) and a TSK-Gel column;
High performance size exclusion chromatography coupled to a multi-angle
laser light scattering detector (HPSEC-MALLS)
Microscopic analysis In situ analysis of pectin structure/location of specific domains by fluorescence
microscopy combined with immunolocalisation by monoclonal antibodies
JIM5 and JIM7
AFM for the analysis of specific regions of pectin following acid hydrolysis
Analysis of morphological changes/optical sectioning by SEM
Other methods Analysis of pectin structure (amorphous or crystalline) by XRD performed on
solid samples (powder form)
Enzymatic digestion of pectin, analysis of the blockwise/nonblockwise
distribution of methylation of GalA by PACE
Blakeney et al. (1983); Müller-Maatsch et al. (2016); Colodel and
De Oliveira Petkowicz (2018)
Kang et al. (2015); Nagel et al. (2017); Guo et al. (2018)
Dische (1946); Wang, Wu, Chantapakul, et al. (2017); Jouini
et al. (2018)
Blumenkrantz and Asboe-Hansen (1973); Abid, Cheikhrouhou,
Renard, et al. (2017); Chaharbaghi et al. (2017); Vasco-Correa
and Zapata Zapata (2017)
Garna et al. (2006); Burana-osot et al. (2010)
Sims and Bacic (1995); Wu et al. (2015); Zhang et al. (2016);
Wang, et al. (2017)
Lin et al. (2016); Georgiev et al. (2017); John et al. (2018)
Savary and Nuñez (2003); Yoo et al. (2012)
Müller-Maatsch et al. (2014); Grassino et al. (2016)
Synytsya et al. (2003); Kyomugasho et al. (2015)
Synytsya et al. (2003); Kumar and Chauhan (2010)
Naghshineh et al. (2016)
Daas et al. (1999); Daas et al. (2000); Sousa, Nielsen, et al. (2015)
Guillotin et al. (2007)
Lira-Ortiz et al. (2014); Jung and Wicker (2014)
Hafrén et al. (2000); Arltoft et al. (2007)
Kirby et al. (2008); Round et al. (2010)
Liew et al. (2014); Zouambia et al. (2017)
Kumar and Chauhan (2010); Sharma et al. (2015); Ponmurugan
et al. (2017); Jiang et al. (2018)
Goubet et al. (2003); Goubet et al. (2005)

the intrinsic properties of pectin determine its physical properties and
contribute to the commercial interest for this soluble fiber (Luz
Fernandez, 2001).
Given the complexity of the multiblock pectin biopolymer, the
analysis of the extracted whole macromolecule does not suffice in
giving insight into the fine structure of pectin. Knowledge on pectin
structure has been largely obtained from chemical-enzymatic analyses
which involve different extraction protocols for sequentially isolating
and characterizing the polymer (Sila et al., 2009). To reveal its struc-
tural characteristics, pectin biopolymer is usually degraded into oligo-
saccharides that are further fractionated to isolate structural elements.
Analytical techniques (Table 4) used to study and quantify the struc-
tural elements of pectin are discussed below.
5.1. Monosaccharide composition and linkage pattern
5.1.1. Sugar composition
Accurate analysis of the carbohydrate composition is particularly
important when studying the structure of pectin polysaccharides, and it
is often desired for monitoring the extraction and purification process
and the quality parameters of the final pectin product. Regarding the
effect of the neutral monosaccharides composition on the technological
applications of pectin, research has shown a positive impact of this
chemical parameter on the formation of pectin gels. A representative
study focused on this matter is the research conducted by Sousa,
Nielsen, Armagan, Larsen, & Sørensen, 2015) on the effect of the
specific reduction in neutral sugars concentration (through controlled
enzymatic debranching) on the rheological properties of high-sugar HM
citrus pectin gels. As explained by the authors, following the decrease in
temperature, chain mobility, and thus the velocity at which new hy-
drophobic interactions are formed in the initial stage of gelling, the
neutral monosaccharides side chains play a key role in further tigh-
tening the gelling network.
In order to determine the neutral monosaccharides content, the
polysaccharides must be first depolymerized into their constituent
sugar residues (uronic acid and neutral monosaccharides), which is
commonly done by chemical or enzymatic hydrolysis. Most of the
methods available for the determination of neutral monosaccharides
involve the use of chromatographic techniques. A simple chromato-
graphic method was described by Blakeney, Harris, Henry, and Stone
(1983) and is based on the determination of alditol acetate derivati-
zation products of the monosaccharides contained in the pectin sample
by gas chromatography. In a first step, monosaccharides are reduced
with a solution of sodium borohydride in dimethyl sulfoxide; an acet-
ylation step then follows, where 1-methylimidazole is added as the
catalyst. The resulting alditol acetates are completely separated in a
chromatographic system equipped with a glass-capillary column. This
method was employed in newer research on the chemical analysis of
pectin from various sources including apple and citrus (Kaya et al.,
2014; Wang et al., 2014). Other variations of the gas chromatographic
method involve flame ionization detection (GC-FID) (Garna et al.,
2007) or mass spectrometric detection (GC-MS) (Colodel & De Oliveira

339
F. Dranca, M. Oroian
Petkowicz, 2018; Müller-Maatsch et al., 2016), which is one of the most
frequently used methods for the analysis of neutral monosaccharide
composition.
In several studies, high performance anion exchange chromato-
graphy with pulsed amperometric detection (HPAEC-PAD) was used to
examine the sugar composition of pectin (Christiaens et al., 2015; Guo
et al., 2018; Kang et al., 2015; Nagel et al., 2017). Kang et al. (2015)
reported on the use of ultrafiltration prior to quantification, in order to
remove impurities such as pigments, salts, acids, and saccharides from
the extracted pectin sample. Willför et al. (2009) conducted a com-
parison between commonly used methods for hydrolysis and sub-
sequent analysis of the released monosaccharides: gas chromatography
(using capillary columns and flame ionization detection and/or mass
spectrometric detection), HPAEC-borate technique, and HPAEC-PAD.
Based on the results it was concluded that gas chromatographic analysis
preceded by a combined acid hydrolysis and methanolysis is a con-
venient method for obtaining the composition of monosaccharides.
Another technique examined for the determination of monosaccharides
present in pectin was centrifugal partition chromatography. Ward,
Cárdenas-Fernández, Hewitson, Ignatova, and Lye (2015) evaluated the
efficiency of a highly polar two-phase system containing ethanol and
aqueous ammonium sulfate for the separation of neutral mono-
saccharides (L-rhamnose, L-arabinose, D-galactose, and D-galacturonic
acid) of hydrolyzed sugar beet pectin. Dimethyl sulfoxide was selected
as an effective phase system modifier improving monosaccharide se-
paration; in the combined form ethanol:dimethyl sulfoxide:aqueous
ammonium sulfate (0.8:0.1:1.8, v:v:v) the system enabled the separa-
tion of monosaccharides by centrifugal partition chromatography in an
ascending mode.
5.1.2. Galacturonic acid content
In order to analyze the galacturonic acid content, pectic substances
must be first hydrolyzed to uronic acid and neutral monosaccharides.
Several procedures have been developed to hydrolyze pectin, most of
them involving the use of concentrated acids or enzymes. All these
methods were reported to present some drawbacks and call for im-
provement; acid hydrolysis requires prolonged treatment and can cause
a degradation of galacturonic acid which ultimately leads to a low re-
covery (Garna, Mabon, Wathelet, & Paquot, 2004), while the other
method requires different types of enzyme activities such as pectolytic,
hemicellulolytic, and carbohydratases for an efficient degradation of
pectin. Despite this drawback, enzymatic hydrolysis is considered a
better technique for the hydrolysis of pectin.
Several colorimetric methods are available for the quantitative
analysis of galacturonic acid. Among spectrophotometric analytical
techniques, carbazole-H2SO4 reaction is one of the early methods of
determination which have been described and later modified by various
other authors. The method was first proposed by Dische (1946) and is
based on the color reaction between the degradation products of pectin
hydrolysis with concentrated acid and carbazole; the resulting colora-
tion is proportional to the concentration of galacturonic acid. In recent
studies, the carbazole method was used to determine the galacturonic
acid content of polysaccharides from Opuntia microdasys var. rufida
cladodes (Jouini et al., 2018) and pectin extracted from waste grape-
fruit peels (Wang, Wu, Chantapakul, et al., 2017) A modification of
Dische's carbazole reaction for uronic acid in the presence of borate was
later described by Bitter and Muir (1962) who noted that the ad-
vantages of this method were the increased sensitivity, greater re-
producibility, and reduction of interference by chloride ion and oxi-
dants. This modified carbazole assay was used by Yeoh, Shi, and
Langrish (2008) for the determination of galacturonic acid content of
pectin from orange peels, by Zhang et al. (2013) in the analysis of
physicochemical properties of polysaccharides obtained from Flammu-
lina velutipes, and by Romdhane et al. (2017) to analyze the uronic acid
content of polysaccharides from watermelon rinds. In their research,
Yeoh et al. (2008) considered the removal of neutral carbohydrates
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Food Research International 113 (2018) 327–350
from the sample a requirement in ensuring that this method is an ac-
curate colorimetric assay to quantify the amount of pectin. The pre-
sence of non-uronide carbohydrates (such as starch, cellulose, and
neutral sugars) in the pectin extract was shown to interfere in the
analysis of galacturonic acid, since the carbazole assay stimulates any
neutral sugar molecules present to form additional color. Similar
methods to the carbazole reaction are the m-hydroxydiphenyl sulfuric
acid assay (Blumenkrantz & Asboe-Hansen, 1973) and the 3,5-di-
methylphenol sulfuric acid reaction (Scott, 1979). Both methods are
characterized by a high specificity for uronides and less sensitivity to
the presence of neutral sugars; an exception was observed for the m-
hydroxydiphenyl sulfuric acid assay when non-uronide carbohydrates
were contained by the sample in high concentrations (Sila et al., 2009).
The m-hydroxydiphenyl reaction, which has become a common method
for the determination of uronic acids, was widely applied in the last
years for the analysis of pectin from various plant sources (Abid,
Cheikhrouhou, Renard, et al., 2017; Chaharbaghi, Khodaiyan, &
Hosseini, 2017; Vasco-Correa & Zapata Zapata, 2017). A method that
avoids the use of concentrated acids commonly needed in the colori-
metric determination with m-hydroxydiphenyl was proposed by Anthon
and Barrett (2008) who described it as a simple procedure for de-
termining the galacturonic acid that relies on enzymatic pectin hydro-
lysis and colorimetric quantification (using arsenic containing the
Nelson reagent). Application of the determination procedure was
evaluated for both soluble and insoluble pectins from apple, oranges,
and several tomato products.
The literature also contains several gas and liquid chromatographic
techniques that were developed to determine the content of uronic acid
in pectin (Garleb, Bourquin, & Fahey, 1991; Ford, 1982; Jones &
Albersheim, 1972); although these techniques indicated promising ap-
plications, they resulted in lower quantification. An accurate analysis of
uronic acids without any derivatization was obtained by Garna, Mabon,
Nott, Wathelet, and Paquot (2006) using HPAEC-PAD. When the
HPAEC-PAD assay was preceded by a combined chemical and enzy-
matic hydrolysis with Viscozyme L9, a major advantage for detection,
namely the liberation of galacturonic acid without any degradation,
was observed. Moreover, the method is selective and sensitive and
provides better accuracy and repeatability. Burana-osot,
Soonthornchareonnon, Chaidedgumjorn, Hosoyama, and Toida (2010)
developed a simple and rapid analytical method based on converting
GalA in the polysaccharide chain into the stable neutral sugar Gal
(preventing decomposition of urinate residues) prior to hydrolysis with
trifluoroacetic acid and analysis of the hydrolysate by HPAEC with
fluorescence detection. By comparison to HPAEC-PAD, the galacturonic
acid content determined with the proposed method was higher, and the
results showed good linearity, high precision, and high sensitivity.
5.1.3. Glycosidic linkage conformation
For a detailed structural characterization of pectin polysaccharides,
the investigation into monosaccharide composition can be completed
with a determination of the positions of the glycosidic linkages by
which the monosaccharide units are connected in polysaccharides. The
distribution pattern of glycosidic linkages in the RG backbone de-
termines the technological applications through the changes in pectin-
water interactions, given the fact that the cleavage of these linkages, as
side reaction of pectin demethoxylation, can lead to reduced water
sorption of the resulting LMP (Einhorn-Stoll, 2018).
The most common methods for carbohydrate linkage analysis are
exoglycosidase (EC 3.2.1.37) digestion, methylation analysis (both in-
volving GC techniques), mass spectroscopy, and nuclear magnetic re-
sonance (NMR) spectroscopy (Bertozzi, Freeze, Varki, & Esko, 2009). Of
these analytical approaches, methylation analysis is viewed as the most
important single method which quantifies all the modes of linkage of
the monosaccharide residues in the polysaccharide (BeMiller, 1996).
The general procedure, as described by Sims and Bacic (1995), is based
on the methylation-induced cleavage of the glycosidic linkages in the
F. Dranca, M. Oroian
native oligosaccharide and the conversion of the resulting partially
methylated individual monosaccharide residues to alditol acetates
(partially methylated alditol acetates, PMAAs) that are separated on a
GC column. The results of the quantification of PMAAs by GC-MS re-
ported in some studies, including those belonging to Wu, Zhang, Yu,
Lin, and Yang (2015), Zhang, Wang, Lai, and Wu (2016) and Wang,
Yang, Zhao, Lu, & Zhu (2017), showed that correct identification of
derivatives and the sugars they are derived from requires both retention
time and mass fragmentation data (Sims, Carnachan, Bell, & Hinkley,
2018). A drawback of this method is that glycosidic linkages adjacent to
uronic acids are not detectable as alditol acetate unless they are pre-
reduced to their neutral sugar counterparts (Pettolino, Walsh, Fincher,
& Bacic, 2012).
Glycosyl linkage analysis has been applied to elucidate the structure
of pectin from various plant matrixes, including the recent use in the
analysis of pectin from flowers of Lonicera japonica conducted by Lin
et al. (2016), who used methylation in combination with NMR analysis
(1H NMR, 13C NMR spectra and 2D spectra). Identification of glycosidic
linkage and side chain location by 1D and 2D NMR was also reported in
structural studies of arabinan-rich pectic polysaccharides from Abies
sibirica L. (Shakhmatov, Toukach, Michailowa, & Makarova, 2014),
water-soluble polysaccharides in papaya during ripening (John, Yang,
Liu, Jiang, & Yang, 2018), and pectins from Tilia tomentosa (Georgiev
et al., 2017). Characteristic signals in 1D and 2D NMR provide in-
formation related to pectin structure. For example, in regards to the
assignments of 1H and 13C NMR chemical shifts, the predominant signal
at 100.4-105.2/4.60-4.63 ppm was assigned to C-1/H-1 of galacturonic
acid β(1→4)-linked (Kienteka, Corrêa-Ferreira, & de Oliveira
Petkowicz, 2018; Shakhmatov et al., 2014), while the correlation peak
C-1/H-1 at 99.1-102.2/5.03 was due to 1,4-α-D-GalpA residues (John
et al., 2018; Shakhmatov et al., 2014).
5.2. Degree of substitution
The functional properties of pectin in food, the reactivity towards
calcium and other cations and, therefore, its potential for cross-linking
is mostly dependent on the amount of non-esterified GalA subunits and
their distribution pattern within the HG chain. The degree of ester-
ification influences physical properties such as surface tension, emul-
sification capabilities (Lutz, Aserin, Wicker, & Garti, 2009) and gel
formation (Yoo, Fishman, Hotchkiss, & Hyeon, 2006). In regards to
gelation, pectin with a degree of methylation above 50% can form gels
at low pH and high sugar concentrations, whereas for pectin with a
methyl esterification degree below that level the gelation is dictated by
the reaction with calcium (May, 1990). Acetylation, like methylation, is
well known to strongly alter pectin associative properties by decreasing
the affinity of HG domains for cations (Ralet, Lerouge, & Quéméner,
2009; Renard & Jarvis, 1999).
Various analytical methods have been described in the literature to
determine the degree of esterification of pectin samples isolated from
diverse plant materials. Most methods are based on using alkaline hy-
drolysis to release methoxyl groups from the galacturonic acid by in-
cubation with sodium hydroxide solution; the methanol content can
then be determined using chromatography, spectrophotometric
methods or FT-IR spectroscopy. Klavons and Bennett (1986) improved
the colorimetric method proposed by Wood and Siddiqui (1971) by
shortening the oxidation time through the use of alcohol oxidase as
replacement for potassium permanganate. In a later study, Anthon and
Barrett (2004) found alcohol oxidase (EC 1.1.3.13) in conjunction with
Purpald (4-amino-3-hydrazino-5-mercapto-1,2,4-triazole) more sensi-
tive to the released methanol. Compared to spectrophotometric tech-
niques, the major advantage of chromatography is that it allows the
separation of impurities prior to the quantification. Efficient separation
and good reproducibility was reported for head-space gas chromato-
graphy (Huisman, Oosterveld, & Schols, 2004) and ion-exclusion
chromatography (Luzio & Cameron, 2013). Another technique
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validated as a method for the routine analysis of the degree of methyl-
esterification was Fourier transform infrared (FT-IR) spectroscopy.
Kyomugasho, Christiaens, Shpigelman, Van Loey, and Hendrickx
(2015) showed that when using FT-IR for the analysis of DM of a pro-
tein-rich sample, such as pectin from broccoli, the peak deconvolution
is vital to correct interferences due to the presence of proteins and to
improve the determination accuracy.
Research on the simultaneous determination of methylation and
acetylation degree of pectin is limited and mostly involves quantifica-
tion using chromatographic techniques such as HPLC (Levigne,
Thomas, Ralet, Quemener, & Thibault, 2002) and GC-MS (Savary &
Nuñez, 2003). By performing a base-hydrolysis of esters and acidifica-
tion of pectin samples, followed by headspace solid-phase micro-
extraction and, finally, analysis of the resulting methanol and acetic
acid by GC-MS, as described by Savary and Nuñez (2003), Yoo et al.
(2012) determined the methyl and acetyl substitution levels in pumpkin
pectin extracted by microwave heating. A different approach to this
matter was taken by Müller-Maatsch, Caligiani, Tedeschi, Elst, and
Sforza (2014) who developed a 1H NMR (proton nuclear magnetic re-
sonance) method that allowed the detection of methylation, acetyla-
tion, and feruloylation degrees of pectin after an alkaline saponifica-
tion. This method can be applied to pectic polysaccharides originating
from a wide range of sources and having different physical properties
and can detect small amounts of methanol, acetic acid, and ferulic acid.
Reports on the use of the 1H NMR method indicated a sharp singlet at
3.75 ppm, which corresponds to protons in the methoxy group of es-
terified galacturonic acid, and chemical shifts at 2.01-2.17 ppm, at-
tributed to the acetyl groups binding at O-2 and O-3 of galacturonic
acid residues (Gopi, Kanimozhi, Bhuvaneshwari, Indira, & Kavitha,
2014; Grassino et al., 2016). Simultaneous determination of methyla-
tion and acetylation degree of pectin can be also achieved using FT-
Raman and FT-IR, as described by Synytsya, Čopı́ková, Matějka, and
Machovič (2003). According to their observations, the very intense
Raman band at 857 cm−1 is sensitive to the state of uronic carboxyls
and O-acetylation, decreasing to the minimum of 850 cm−1 with the
degree of substitution by methyl groups and increasing (to max. 862
cm−1) with acetylation. Low intensity Raman bands at 1164, 1184 and
1471 cm−1 were attributed to acetylation of pectin samples (Kumar &
Chauhan, 2010). Other research that must be mentioned here is the
environmentally friendly method for the automated determination of
pectin DE using the μSI-LOV system developed by Naghshineh, Larsen,
Georgiou, and Olsen (2016). The determination proved to be fairly
simple, precise, reproducible, and economical.
5.3. Degree of blockiness
As was mentioned before, the degree and pattern of methyl-ester-
ification influences the functional properties of pectin; because of its
effect on gel-forming and rheological properties, the commercial im-
plications of DE have been extensively studied. As a way to describe the
percent of non-esterified GalA units present in pectin, expressed as the
blockwise distribution of the free carboxyl groups, Daas, Meyer-Hansen,
Schols, De Ruiter, and Voragen (1999) introduced the term degree of
blockiness (DB). The degree of blockiness is an important parameter for
the retention of water in pectin gels and influences, to a lower extent,
the water uptake of pectin powders (Einhorn-Stoll, 2018). Studies
showed that, when compared to pectin samples with randomly dis-
tributed carboxyl groups, HMP with partly blockwise distributed free
carboxyl groups displayed increased water uptake and later dissolution
(Einhorn-Stoll, Benthin, Zimathies, Görke, & Drusch, 2015). Daas et al.
(1999) described a method used to determine the degree of blockiness,
which was based on the analysis of the oligomers released after pectin
digestion with endopolygalacturonase (EC 3.2.1.15) from Kluyver-
omyces fragiles, their separation and quantification using HPAEC at pH
5. Determination of DB by HPAEC-PAD method (Daas et al., 1999; Daas,
Voragen, & Schols, 2000) was important for the investigation of pectin
F. Dranca, M. Oroian
rheological behavior and the study on the effect of pectin properties on
coacervates formation with pea protein isolate (Sousa et al., 2015;
Warnakulasuriya, Pillai, Stone, & Nickerson, 2018). A similar procedure
for the separation of oligomers, involving digestion of pectin with en-
zymes, followed by analysis using capillary electrophoresis (CE) for the
determination of the degree of blockiness of several commercial pec-
tins, was reported by Guillotin, Bakx, Boulenguer, Schols, and Voragen
(2007). The CE method was found to present two main advantages by
comparison to other quantification methods available up to that point:
the very low amount of sample required, especially when compared to
HPAEC and the possibility to simultaneously analyze the oligomers and
polymers from the polygalacturonase digest.
While the above-mentioned methods give good results, other tech-
niques found in the literature have proved not to be accurate for the
determination of DB. When applying 1H NMR for the quantification of
the degree of blockiness of pectin, Winning, Viereck, Nørgaard, Larsen,
and Engelsen (2007) observed that the H-1 signal strongly covariated
with random deesterification, but not with blockiness. As a result, it
was concluded that the proposed method was better suited for the
prediction of random deesterification rather than the determination of
the degree of block deesterification. Lack of specificity for the char-
acterization of DB was also indicated by Sousa, Ahl, et al. (2015) who
took a multivariate analysis approach with the purpose to analyze a set
of pectin samples probed with 14 different monoclonal antibodies. In
their study the development of partial least squares models allowed
prediction of DM values in an accurate form, but at the same time was
not good enough for the prediction of DB.
5.4. Molecular weight
Early research on the application as gelling, thickening, and stabi-
lizing agents showed that the performance of pectin is critically de-
pendent on the average molecular weight and the distribution of mo-
lecular weights. For example, by studying the effect of chemical
composition on the compressive mechanical properties of low-ester
pectin gels it was observed that preparations with molecular weight
distributions possessing broad low-molecular-weight tails yielded poor
gelling properties (Kim, Rao, & Smit, 1978). A method to increase
pectin calcium sensitivity, while preserving its molecular weight that
has been evaluated, is enzymatic modification. The analysis conducted
by Hotchkiss et al. (2002) on the deesterification of citrus pectin with a
purified salt-independent PME revealed no reduction in average mole-
cular weight, in contrast to alkali deesterification that caused a rapid
reduction of both molecular weight and intrinsic viscosity. The same
major influence of molecular weight was not uncovered in emulsifica-
tion experiments. By researching the emulsification properties of citrus
pectin Schmidt et al. (2015) reached the conclusion that pectins with a
reduced molecular weight do neither significantly reduce droplet sizes
nor improve emulsion stability.
The molecular weight distribution of pectins is generally de-
termined by chromatographic techniques. Early analytical methods
were developed on citrus pectin samples and were based on the use of
gel permeation chromatography (GPC) (Berth, Dautzenberg, Lexow, &
Rother, 1990; Harding, Berth, Ball, Mitchell, & de la Torre, 1991). A
more recent application of GPC to determine the molecular weight of a
purified fraction of polysaccharide from mulberry leaves was described
by Ying, Han, and Li (2011). The researchers combined GPC with a
HPLC instrument equipped with an Ultrahydrogel column. This method
was later employed to determine the molecular weight of samples of
citrus and apple pectin (Wang et al., 2014). Other variations of the
chromatographic method involved the determination by high-perfor-
mance size-exclusion chromatography (HPSEC) equipped with two
columns in series (Lim, Yoo, Ko, & Lee, 2012) or a TSKGel column (Lira-
Ortiz et al., 2014) and a refractive index detector (HPSEC-RID), high
performance size exclusion chromatography coupled to a multi-angle
laser light scattering detector (HPSEC-MALLS) (Jung & Wicker, 2014),
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Food Research International 113 (2018) 327–350
high performance gel filtration chromatography with refractive index
detector (Hua, Yang, Din, Chi, & Yang, 2018), and a HPLC system
equipped with a TSKgel column coupled on-line with three detectors – a
differential refractometer that measures the refractive index, a right-
angle laser light-scattering detector, and a differential viscometer de-
tector (Combo et al., 2013). Of these chromatographic methods, HPSEC
coupled to MALLS or RID work well for pectin from various sources
(Kang et al., 2015; Karnik, Jung, Hawking, & Wicker, 2016; Kienteka
et al., 2018; Liu, Guo, Liang, Liu, & Chen, 2017). A recent evaluation of
the evaporative light scattering (ELS) and refractive index detectors
coupled to HPSEC and comparison in terms of molecular weight esti-
mation on commercial pectin samples, in a wide range
(0.342–805 kDa), led to the conclusion that HPSEC-ELS gives better
results for low molecular weight compounds (Muñoz-Almagro, Rico-
Rodriguez, Villamiel, & Montilla, 2018).
The average molar weight of pectin samples can also be estimated
using the Mark-Houwink equation (Eq. (1)), as described by Arslan
(1995):
η = K × Ma (1)
−1
where K (L∙g ) and a are constants (K=0.0436 and a=0.78), M
(g∙mol−1) is the molecular weight, and η (L∙g−1) is the intrinsic visc-
osity defined according to Eq. 2.
ηr − 1
[η] = lim ⎛ ⎞
C→0 ⎝ C ⎠ (2)
−1
where ηr is relative viscosity and C (g∙L ) is pectin concentration.
Based on the Mark-Houwink equation and using a Cannon-Fenske
capillary viscometer for the measurement, Venzon et al. (2015) de-
termined the molecular weight of modified pectin extracted from or-
ange pomace, while Urias-Orona et al. (2010) applied the relationship
between intrinsic viscosity and molecular weight to characterize
chickpea husk pectin.
5.5. Microscopic analysis
With the development of microscopic techniques more information
about the structure of the cell wall and its components could be col-
lected. The visualization of pectin isolates from various plant materials
can provide data regarding the content of galacturonic acid and the
distribution of GalA residues, the position of glycosidic linkages in
pectic chains, the degree of esterification, the localization of esterified
groups, the molecular weight distribution pattern, and profile of the
neutral monosaccharides.
In the particular case of fluorescence microscopy, the progress in the
application of this technique prompted the increase of research on the
use of fluorescent markers with defined excitation and emission spectra
as specific labels of cellular functions (Sila et al., 2009). When ana-
lyzing cell wall components, specific staining or immunolabeling
techniques are generally used. Van Der Veen and Van Den Ent (1994)
applied immunolocalization with a fluorescent pectin probe, specific for
a block of at least 16 subsequent homogalacturonic units, and they
showed that the middle lamella of Populus deltoids (eastern cottonwood)
contains pectin polysaccharides. In the same study, staining with ru-
thenium red indicated the presence of pectin in both ray parenchyma
cell walls and the middle lamella area of Populus deltoids and Pinus
sylvestris (Scots pine). With the introduction of JIM5 and JIM7 anti-
bodies, research on the spatial distribution and the relative amount of
acidic and methylated pectin present in various plant tissues was made
possible (Casero & Knox, 1995; Knox, Linstead, King, Cooper, &
Roberts, 1990). Immunocytochemical localization of pectin by JIM5
and JIM7 monoclonal antibodies has shown great enhancement of
specificity in detection. This conclusion was corroborated by Hafrén,
Daniel, and Westermark (2000) who immunolocalized HGs with low
and high degrees of methyl esterification in the cambium, differ-
entiating xylem and mature xylem of Pinus sylvestris. Outside plant
F. Dranca, M. Oroian
material, JIM5 antibody has been successfully used for in situ locali-
zation of pectin in yogurt and model milk gels (Arltoft, Madsen, &
Ipsen, 2007). A set of monoclonal antibodies (LM18, LM19, and LM20)
with a better defined HG epitope was later developed by
Verhertbruggen, Marcus, Haeger, Ordaz-Ortiz, and Knox (2009).
Atomic force microscopy (AFM) is a powerful imaging technology
with an increased number of applications in the study of pectin isolates.
Because it can produce subnanometer-scale images of individual mo-
lecules, AFM has proved to be a useful tool for the characterization of
complex samples. By studying the images obtained following an AFM
analysis of isolated polymers, some researchers reported on the struc-
ture and degree of branching of pectin. Notable studies include visua-
lization of the structures of pectin molecules isolated from unripe to-
mato, which concluded in the finding that the complex biopolymer
consists of HGs held together by RG-I regions (Round, Rigby,
MacDougall, & Morris, 2010). AFM was also used in the analysis of
pectin isolated from sugar beet tissue, and it revealed the presence of
largely un-aggregated chains: a major fraction (67%) was poly-
saccharide-protein complexes containing a single protein molecule at-
tached to one end of the polysaccharide chains, and a small fraction
(33%) of these was extended stiff polysaccharide chains (Kirby,
MacDougall, & Morris, 2008). Besides information regarding the
branching of pectin chains, atomic force microscopy was successfully
employed as a mean to distinguish between pectins from different
peach cultivars (Yang, Chen, An, & Lai, 2009).
Another technique that found great application in recent studies on
pectin extracted from various plant materials is scanning electron mi-
croscopy (SEM). Liew et al. (2014) used this microscopic technique to
elucidate the morphological changes of pectin samples which were
extracted by an acidic extraction method from passion fruit peel, while
Zouambia, Youcef Ettoumi, Krea, and Moulai-Mostefa (2017) per-
formed a SEM analysis on alcohol-insoluble solids before and after ex-
traction in order to visualize the effect of heating mode on the de-
struction of plant tissue used for the extraction of pectin. By combining
scanning electron microscopy with atomic force microscopy,
Zhongdong, Guohua, Yunchang, and Kennedy (2006) researched the
process of pectin extraction from orange skin assisted by microwave
energy. Morphological analysis using scanning electron microscopy was
reported for samples of pectin from pomelo peel (Liew et al., 2016) and
raw and treated jackfruit peel (Moorthy et al., 2017), and also for
biodegradable matrices composed of a pectin network reinforced by a
poly(lactide-co-glycolide) network (Liu et al., 2004).
5.6. Other methods
More information regarding pectin structure (amorphous or crys-
talline) can be obtained by X-ray diffraction (XRD) analysis (Jiang, Du,
Zhang, & Li, 2018; Sharma, Kamboj, Khurana, Singh, & Rana, 2015).
Similar to all polymers, pectin presents some degree of crystallinity,
which has been defined as the fraction of a polymer that consists of
regions showing three-dimensional order (Riley, 2012). Based on the
peaks displayed on the diffraction patterns, Ponmurugan et al. (2017)
observed a parallel crystalline nature (sharp and narrow diffraction
peaks) in both commercial pectin and pectin extracted from sunflower
waste, while Kumar and Chauhan (2010) concluded that pectin ex-
tracted from the commercial Royal apple was more crystalline in nature
than pectin extracted from Golden apple variety. Another analytical
technique that can be used to differentiate between pectin samples is
gel electrophoresis. Polysaccharide analysis using carbohydrate gel
electrophoresis (PACE) is a method proposed for studying the blockwise
or nonblockwise distribution of methylation of galacturonic acid re-
sidues by analyzing the endopolygalacturonase-digest products
(Goubet, Morriswood, & Dupree, 2003; Goubet, Ström, Dupree, &
Williams, 2005). Other analytical methods used to investigate the
properties and behavior of pectin samples are discussed below.
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5.6.1. Thermal analysis
Based on the fact that carbohydrates show first-order phase transi-
tions (such as melting and crystallization) and state transitions (such as
gelatinization and glass transition), thermal analysis proved to be a very
useful and rapid screening method for the characterization of pectin
(Einhorn-Stoll, Kastner, & Senge, 2012; Roos, 2003). Thermal analysis
techniques, such as dielectric analysis, differential scanning calorimetry
(DSC), and thermogravimetry analysis (TGA), can provide insight into
the physicochemical properties of the biopolymer. Lin, Yuen, and
Varner (1991) used differential scanning calorimetry to study the phase
transition of cell wall preparations, and they reached the conclusion
that the mature region of soybean hypocotyls either has more calcium
in the wall or has more methyl-esterified pectin, which makes it less
responsive to calcium addition. Using differential scanning calorimetry,
thermogravimetry, and differential thermogravimetry (DTG) in a
combined simultaneous thermal analysis, Einhorn-Stoll, Kunzek, and
Dongowski (2007) aimed to investigate the thermal behavior of highly
methoxylated citrus pectins that were modified chemically (de-
methoxylation and amidation) and mechanically (disaggregation).
Their results showed that thermal behavior of pectin is considerably
influenced by the physical state, resulting both from different raw
materials and modifications of the molecular structure (different sub-
stituents or decreasing molecular weight). In a later study Einhorn-Stoll
and Kunzek (2009) concluded that the characteristic degradation
temperatures along with other parameters of thermal analysis give
important information on the stability, homogeneity, molecular inter-
actions, conformation, and conformational changes, the latter two as-
sumed to be detectable by thermal analysis to a certain extent.
Thermal analysis (DSC and TGA with DTG) was evaluated alongside
other analytical methods (chemical analysis, color measurement, SEM,
and FT-IR spectroscopy) for its potential to be used as a screening
method for the characterization of changes occurring in pectin during
storage. For this purpose, Einhorn-Stoll, Kastner, and Drusch (2014)
examined citrus pectin samples that were stored and then analyzed for
alterations in molecular parameters, surface morphology, color, as well
as behavior in thermal analysis. The combination of DSC and TGA
proved to be a valuable instrument for the detection of differences in
stored pectins, as DTG peaks indicated two similar changes in pectin
samples, namely reduced homogeneity (mainly by depolymerization)
and maximum degradation velocity after storage. Other uses of DSC
were to examine the effects of extraction temperature and raw material
on the thermodynamic properties of pectin (Wang et al., 2014), and in
combined TG-DSC to characterize and evaluate pectin and mefenamic
acid films (Moreira, Teixeira, Furuyama-Lima, De Souza, & Siqueira,
2014).
5.6.2. Rheological characterization
Aqueous solutions of pectin show pseudoplastic non-thixotropic
behavior, independent of the degree of methoxylation, but directly
dependent on the concentration. In other words, the pseudoplasticity of
pectin solutions decreases with decreasing concentration (Visser &
Voragen, 1996). The linear relationship observed between shear stress
and shear rate of pectin solutions indicates Newtonian behavior, but
only below a certain concentration (Fig. 4). According to the literature,
at concentrations higher than 3% (v/v) pectin solutions have non-
Newtonian flow (Iagher, Reicher, & Ganter, 2002); however, it is im-
portant to be mentioned that the actual critical concentration at which
the solution transforms from Newtonian to shear-thinning behavior
depends on the molecular weight of pectin (Chan et al., 2017).
Lira-Ortiz et al. (2014) studied the rheological properties alongside
the chemical characteristics of pectic polysaccharides extracted from
the peel of prickly pear fruit (Opuntia albicarpa Scheinvar ‘Reyna’) with
the purpose to assess their potential as new food hydrocolloids. The
aqueous pectin systems in the range of 5-20 g/kg exhibited shear-
thinning behavior over the shear rate range examined, while the visc-
osity values were higher when compared to citrus pectin dispersion.
F. Dranca, M. Oroian Food Research International 113 (2018) 327–350

Fig. 4. Viscosity as a function of shear rate for pectin solutions at concentrations of 1–13% (A) and 1–30 g L–1 (B) revealing Newtonian behavior at concentrations
below 3% and pseudoplastic behavior at concentrations above this level (Sousa, Nielsen, et al., 2015; Iagher et al., 2002).

The high viscosities and shear-thinning behavior exhibited by the
aqueous dispersions were mainly explained by the high molecular
weight of the polysaccharide. Moreover, the authors noted that the
likely branched structure of prickly pear fruit pectin, mainly formed by
side chains of oligosaccharides, suggests that the shear flow behavior of
pectin in aqueous dispersions was due to increasing physical en-
tanglements among chains as polymer concentration increased, which
were then disrupted at higher shearing, thus yielding shear-thinning
behavior. The influence of pectin chain branching was also confirmed
by Sousa, Nielsen, et al. (2015) who studied the effects of controlled
enzymatic debranching on structural and rheological properties of HM
citrus pectin, and the possible implications of RG-I side chains. They
reported that for all the analyzed concentrations debranched pectin
solutions displayed lower viscosities. In the particular case of
pomegranate Abid, Cheikhrouhou, Cuvelier, et al. (2017) observed that
the rheological properties of peel gels result from a strong synergism
between fibrous material and pectins. Moreover, mechanical treatment
of fibrous material suspensions was found to also significantly affect gel
strength improvement, probably due to the decrease of particle size and
the heat induced by mechanical treatment.
5.6.3. Functional properties
Pectin is a valuable functional ingredient with food applications that
include the use as gelling agent in jams and jellies, emulsifying agent in
various applications such as flavor, mineral, and vegetable oils emul-
sions, effective stabilizer in fruit juices and acidified milk drinks, and as
fat replacer in ice creams and spreads (Begum, Yusof, Aziz, & Uddin,
2017; Naqash, Masoodi, Rather, Wani, & Gani, 2017). Among pectins,
sugar beet pectin has shown excellent emulsifying properties mainly

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F. Dranca, M. Oroian
due to many factors such as the highly branched polysaccharide
structures, high content of hydrophobic acetyl groups on the GalA
chain, and protein moiety, which plays an important role. Karnik and
Wicker (2018) compared the stability of emulsions prepared with
protein rich and protein poor fractions of SBP by measuring the particle
size, steady stress controlled tests, and visual analysis using dark field
microscopy, and observed that the protein poor fraction, with smaller
particle size, but higher DE and molecular weight was a more effective
emulsifier than the pectin fraction rich in protein. The emulsion sta-
bility was also studied by Juttulapa, Piriyaprasarth, Takeuchi, and
Sriamornsak (2017) with the purpose of analyzing the effect of using
high-pressure homogenization for the preparation of an emulsion con-
taining pectin and zein. The use of this technique was based on the
hypothesis that high-pressure homogenization can cause a decrease of
droplet size below 1 μm, improving the shelf-life of the emulsions by
reducing the creaming rate. Although in the case of this study the
droplet size decrease only slightly, probably due to the high oil content
in the formulation, the emulsions stabilized by HMP-zein, showed good
stability and lower percent of creaming index.
The gelling properties of pectin have been extensively studied along
the years and are the main focus of numerous investigations on the
structure-function relationships of pectin in food. For HMP, which form
gel structures through hydrogen bonding and hydrophobic interactions,
the gelation mechanism is promoted by low pH and water activity, as
well as the presence of a high sucrose concentration. In positive influ-
ence of low pH on pectin gelation was confirmed by Jiang et al. (2012)
in a study on the properties of pectins extracted from Akebia trifoliate
var. australis peel. Textural analysis (hardness, springiness, adhesive-
ness, chewiness, gumminess, cohesiveness, and resilience) performed
on the pectin gels showed a decrease of gelling properties with the
decrease of pH from 4 to 2. In the case of LMP, gelation is promoted by
intrinsic factors such as high GalA content, molecular weight, and DB,
and is influenced by some extrinsic factors including pectin con-
centrations, temperature, pH, type and concentration of soluble solids,
and type and concentration of divalent cations (Kastner, Einhorn-Stoll,
& Drusch, 2017). Of the recent research on the formulation of LMP gels,
the work of Yang et al. (2018) aimed to explore the effects of a wide pH
range (3.5-9.5) on LM apple pectin gelation by analyzing the gel
strengths, rheological properties, thermal stabilities, and crystalline
structures. The results of pectin gelation analysis indicated an increase
of gel strength and gelling rate with the increase of pH from 3.5 to 8.5,
due to the high amount of dissociated carboxylic groups, and a decrease
of gel strength and gelling rate for the pH increase to 9.5, attributed to
the decreasing molecular weight of the pectin. Furthermore, it was
noted that the incorporation of Ca2+ into pectin caused a reduction of
the thermal decomposition rate and the crystalline degree. For dees-
terified pectins, the dependence of pectin gelation on pH and Ca2+ was
found to vary mainly with the change in molecular weight and degree
of methylation (Hua et al., 2018).
6. Concluding remarks and future perspectives
The ubiquitous cell wall component pectin found applications as
emulsifier, gelling, thickening and stabilizing agent that go beyond the
food industry and include various uses in the medical and pharma-
ceutical industries. The last few years have seen with an increase in
pectin research carried out with the purpose to isolate pectin from
various plant materials and to elucidate its structure in order to assign
possible applications. A predominant focus of recent research is to in-
vestigate the composition and the properties of pectin extracted from
alternative sources that, in most part, seem to be represented by wastes
of the fruit and vegetable processing industries. Based on the content of
pectin and its composition, some of the representative sources that have
shown great potential for commercial production of pectin are pomelo
peel and the wastes from tomato and carrot processing, mostly those
generated by the canning industry. To understand their applicability in
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Food Research International 113 (2018) 327–350
commercial pectin production and to establish whether or not these can
be considered sustainable pectin sources, studies on a designed pilot
scale process, such as those published by Andersen et al. (2017) and
Casas-Orozco et al. (2015), are necessary. An important particularity
that also needs to be considered in future studies is the geographical
distribution and the variability in the quantity of these plant wastes.
The present work also reviewed the purification and fractionation
techniques and the methods used in the analysis of physicochemical
properties, therefore giving complete insight into the current state of
research on all the particularities of pectin characterization. Concerning
this matter, it is important to highlight that various techniques have
been applied in the analysis of pectin, and therefore continuous im-
provement is expected to be made in the analytical methods for de-
termining the composition and properties of these cell wall poly-
saccharides, and particularly those that dictate its use in the food
industry.
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