Food Chemistry 351 (2021) 129247

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Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem

Review

Utilization of pomelo peels to manufacture value-added products: A review

Li Xiao a, Fayin Ye a, Yun Zhou a, Guohua Zhao a, b, *
a
College of Food Science, Southwest University, Chongqing 400715, People’s Republic of China
b
Chongqing Engineering Research Centre for Regional Foods, Chongqing 400715, People’s Republic of China

A R T I C L E I N F O A B S T R A C T

Keywords: Pomelo peel as a by-product from pomelo consumption is rich in various nutrients and functional compounds,
Pomelo peel while most of the by-product is disposed as wastes. The utilization of pomelo peels could not only result in
Utilization valued-added products/ingredients, but also reduce the environmental threats. By mainly reviewing the recent
Bioactive components
articles, pomelo peels could be directly used to produce candied pomelo peel, tea, jams, etc. Additionally,
Essential oil
functional components (essential oils, pectin, polyphenols, etc.) could be extracted from pomelo peels and
Pectin
Polyphenol applied in food, pharmaceutical and chemical fields. The extraction methods exerted important influences on the
composition, physicochemical properties, bioactivities and structures of the resultant fractions. Furthermore,
pomelo peel was exploited to make adsorbents, bioethanol, etc. For the future investigations, the functionality- or
bioactivity-oriented regimes to recovery valuable components from pomelo peel should be developed in an
economic, effective and eco-friendly way and their applicability in large-scale production should be addressed.

1. Introduction
Pomelo (Citrus grandis (L.) Osbeck), known as pummelo or shaddock,
belongs to the family Rutaceae and is a commercially important cultivar
of the citrus genus, which is widely cultivated around the world. The
pomelo fruit is one of the most consumed fruits. According to FAO
database, the global harvested area and yield of pomelo (including
grapefruit) were 3.7 × 105 ha and 9.4 × 106 tons in 2018, respectively.
The top five countries in pomelo fruit yield include China (5.07 × 106
tons), Vietnam (6.58 × 105 tons), USA (5.59 × 105 tons), Mexico (4.60
× 105 tons) and South Africa (4.45 × 105 tons), as shown in Supple­
mentary material 1 (FAO, 2018). Besides being as a table fruit, pomelo
fruit is often processed into juice, drinks and cans (Liu, Guo, Cai, Liu, &
Li, 2016; Weng, 2011). In gross, these consumptions result in a large
amount of pomelo peels as a by-product, accounting for approximately
30% ~ 50% (w/w) of the fruit. Roughly estimated, the total world
production of pomelo peels approached 2.8 million tons ~4.7 million
tons in 2018. A typical drawing of pomelo fruit is given in Supplemen­
tary material 2. The chemical analysis showed that fresh pomelo peel is
rich in various nutrients and functional compounds such as dietary fiber,
pectin, essential oils and various polyphenol-dominant phytochemicals
(Supplementary material 3). The major components of pomelo peels
have been evidenced with various health-promoting effects, such as
anti-inflammatory, antitumor, anticlotting, antimicrobial and
antioxidant activities (Lan-Phi & Vy, 2015; Oboh & Ademosun, 2012;
Wang et al., 2017). Thus, the improperly disposed pomelo peels is liable
to be a source of environment pollution due to its high perishability. On
the other hand, the elaborate utilization of pomelo peels can derive a
serial of valued-added products or ingredients for food, cosmetics and
pharmaceutical industries.
In this regard, the comprehensive valorisation of pomelo peels is not
only a key strategy in constructing a sustainable pomelo industry but
also a crucial way to improve its socioeconomic performance. In the last
decade, the comprehensive valorisation of pomelo peels gained a lot of
achievements. Being sugar-pickled, the bitterness of pomelo peels was
successfully masked and the resultant products could serve as candies
(Ma et al., 2014). In contrast, more attempts were made on the efficient
recovery of its diversely functional components from pomelo peels
including essential oils, pectin, polyphenols, coumarins, etc. (Qin, Ngoh,
Yusoff, & Teoh, 2017; Liu, Qiao, Gu, Yang, & Yang, 2017; Zhao, Yang
et al., 2019). To achieve this goal, advanced extraction techniques have
been developed (Tuan, Dang, Huong, & Danh, 2019; Jiang, Shen, & Xia,
2014; Liu, Qiao, Gu, et al., 2017). In addition, applicability of pomelo
peels as an alternative material to produce biomass fuel or adsorbents
was explored (Huang et al., 2014; Zhao, Ying et al., 2018). With aims to
update the state-of-the-art technology, identify the current problems
and propose the perspectives and potential directions of the researches
on pomelo peels, a systematic review was made in present work by

* Corresponding author at: College of Food Science, Southwest University, 2 Tiansheng Road, Chongqing 400715, People’s Republic of China.
E-mail address: zhaogh@swu.edu.cn (G. Zhao).

https://doi.org/10.1016/j.foodchem.2021.129247
Received 28 October 2020; Received in revised form 24 January 2021; Accepted 28 January 2021
Available online 15 February 2021
0308-8146/© 2021 Elsevier Ltd. All rights reserved.
L. Xiao et al.
mainly referencing the publicly released works in last decade.
2. Direct utilization of pomelo peels as a raw food material
The pomelo peels can be used as a raw material in producing pickled
fruits, jams as well as high-dietary-fiber food ingredients. In this way,
fresh or dried pomelo peels was dominantly treated by various physical
approaches and, in the final products, almost all their intrinsic compo­
nents were retained and seldom residues were produced.
2.1. Sugar-pickled pomelo peels
The sugar-pickled pomelo peels were commonly made from the fresh
pomelo peels. It can be consumed as preserved fruits or a candy. In
addition, it was often used as a special flavour enhancer in constituting
the filling of various cakes and wheat/rice dumplings. A typical flow­
chart of sugar-pickled pomelo peels was illustrated in Supplementary
material 4a.
The key procedures include blanching, hardening, debitterization,
sugar permeation and drying. The aim of blanching was to inactivate the
intrinsic enzymes, mainly the pectin lyases. It was operated by cooking
pomelo peel slices in boiling water for about 2 min. The hardening was
carried out by soaking blanched pomelo peels in a CaCl2 solution
(~0.75% w/v), by which insoluble pectin salt formed and it benefited
the hardness of pickled pomelo peels. During the hardening operation,
citric acid (~0.5% w/v) or NaHSO3 (~0.3% w/v) was often added to
prevent possible color deterioration (Ma et al., 2014). The debit­
terization was the most important procedure and usually realized by
cooking the pomelo peels in a boiling saline solution (~3% w/v) for 8
min ~ 12 min, in which most bitter substances in pomelo peels such as
naringin and limonin were extracted into the saline (Weng, 2011). The
traditional sugar permeation was implemented by soaking pomelo peels
in a concentrated sugar solution. In order to accelerate the mass transfer
of sugar into pomelo peels, the peel material was moderately dehydrated
prior to the permeation operation. Commonly, a mixture included su­
crose and converted sugar. Finally, the pickled pomelo peels were dried
to achieve a final total sugar content not less than 60% (w/w), guar­
anteeing its microbial safety during shelf life (Wang, 2015).
In view of the disadvantages existed in the traditional processing, a
serial of novel techniques have been explored to produce sugar-pickled
pomelo peels with improved quality. Firstly, for the adverse effects of
the boiling debitterization on the texture of pomelo peels, several
alternative debitterizing regimes were developed. Li, Liu, Li, Liu, and
Zhou (2013) founded that an excellent debitterization could be achieved
by soaking pomelo peels in β-cyclodextrin solution (0.6 g/100 mL) at
45 ◦ C for 60 min. By this regime, a debitterizing rate of 50.6%, the
removal percentage of total bitter substance from the pomelo peels, was
obtained, which was significantly higher than that of traditional boiling
debitterization. This was possibly due to the capture capacity of
β-cyclodextrin for the liberated bitter substances, decreasing the con­
centration of free bitter substances in soaking solution and further
enhancing mass transfer rate from peel to solution. Alternatively, the
incubating of pomelo peels with naringinase (0.3% w/v) at 60 ◦ C could
attain a more satisfied debitterizing rate up to 79.5%. It was achieved via
the enzymatical conversion of naringn into rhamnose, glucose and
naringenin by naringinase in pomelo peels. In the traditional processing,
sugar permeation was the most time-consuming stage. To improve its
efficiency, a gradient sugar permeation was often adopted. Moreover,
innovative regimes, such as vacuum and ultrasound-assisted perme­
ations have been developed. For vacuum permeation, the sugar
permeation was operated at a pressure about 0.06 MPa (Hu, Xia, & Peng,
2002). For ultrasound-assisted permeation, it was proved that, in
contrast to the traditional soaking method, a comparable permeation
could be by assisting the permeation process with 300-W ultrasound at
60 ◦ C for 30 min (Liu, Zhuang, & Shang Guan, 2019). In view of the high
sugar content and high calory of the traditional sugar-pickled pomelo
2
Food Chemistry 351 (2021) 129247
peels, a novel and healthier product was developed by Xia, Liao, Cheng,
and Lu (2010) by substituting the sucrose with xylitol, an energy-free
food sweetner.
2.2. Honey-pomelo tea
Honey-pomelo tea referrs to the canned honey-sweetened pomelo
peels with or without pomelo pulp (Supplementary material 4b). Its
“tea” name is given in considering its consuming way like Chinese tea.
Specifically, the honey-pomelo tea is mixed with boiling water and the
resultant soup consumed as a drink. Instead of the hardening operated in
the processing of sugar-pickled pomelo peels, a softening procedure was
implemented in the production of honey-pomelo tea. It was often per­
formed simultaneously with the debittering procedure by cooking the
peel in a boiling saline solution (Liu et al., 2016). For the product con­
taining the pulp, the homogenized pulp was used together with a
thickener. Usually, both honey and sucrose were used as sweeteners in
honey-pomelo tea. However, the dosages of involved ingredients,
including peel, pulp, sucrose, honey, varied from product to product. For
its safe preservation in shelf life, the canned honey-pomelo tea was often
sterilized by incubating in a hot water bath (>80 ◦ C) for 15 min.
2.3. Jams with pomelo peels
In the aforementioned products, the size-differed pieces of pomelo
peels were applied. Moreover, the debitterized pomelo peels can be
homogenized into a fine slurry. The resultant slurry, with or without
mixed with other fruit or vegetable juices, can be formed in a jam
showing a pomelo flavor (Yuan & Yang, 2009). At least, the pomelo peel
slurry was successfully used in making pineapple and carrot jams (Hai,
Tong, & Lu, 2011; Yuan & Yang, 2009).
2.4. Wholemeal of pomelo peels
The wholemeal of pomelo peels was made from dry debitterized
pomelo peels by various micronization techniques. The dietary fiber was
the major component of pomelo peel wholemeal accounting for
approximate 70% (w/w, db). Thus, it was commonly used as an ingre­
dient to make high-dietary-fiber foods. The pomelo peel wholemeal was
characterized with excellent water- and oil-holding capacities and
swelling capacity (Wang et al., 2014). When pomelo peel wholemeal
was incorporated below 10% (w/w), the resultant rice noodles pre­
sented significantly higher cooking weight (136% ~ 166%) in contrast
to the control sample (125%). However, regardless of its incorporation
level, the pomelo peel wholemeal deteriorated the elongation of the
noodles (Wandee et al., 2014). More interestingly, a health beneficial
rice noodles with a total dietary fiber content of 14.4% (w/w) was
successfully developed by adding the mixture of cassava pulp and
pomelo peel wholemeal (80%:20%, w/w). In contrast to the control
noodles, the obtained rice noodles displayed a higher cooking weight
and comparable tensile stress and elongation. Similar trends were
observed on fresh wheat noodles (Ji, Ji, Fu, & Zhang, 2017). When
pomelo peel wholemeal was enriched into bread, the product hardness,
chewiness, elasticity and adhesiveness increased with the wholemeal
addition and the optimal addition was concluded as 12% (w/w) in terms
of the consumer acceptability (Luo & Xie, 2019).
3. Fractionization of functional ingredients from pomelo peels
3.1. Essential oils from pomelo peels
3.1.1. Major constituents in pomelo peel essential oils
As showed in Supplementary material 3, the level of essential oils in
pomelo peels varied from 204 mg/100 g to 3119 mg/100 g, which was
similar to those in other citrus peels, such as C. reticulata (151 mg/100 g
~ 6837 mg/100 g), C. sinensis (508 mg/100 g ~ 2543 mg/100 g), C.
L. Xiao et al. Food Chemistry 351 (2021) 129247

limon (741 mg/100 g ~ 3164 mg/100 g) and grapefruits (457 mg/100 g
~ 1774 mg/100 g) (González-Mas, Rambla, López-Gresa, Blázquez, &
Granell, 2019). The chemical analysis revealed that pomelo peel
essential oils was mainly constituted by monoterpene hydrocarbons
(78.19% ~ 99.54%) and sesquiterpene hydrocarbons (≤2.09%) as well
as their oxygenated derivatives (≤9.65%) (Table 1). In the subgroup of
monoterpene hydrocarbons (C10H16), limonene (43.84% ~ 96.71%),
myrcene (≤39.3%), γ-terpinene (≤13.50%), sabinene (≤4.22%),
β-pinene (≤3.16%) and α-pinene (≤3.28%) were frequently identified.
The sesquiterpene hydrocarbon subgroup (C15H24) was mainly
comprised of β-cubebene (≤1.52%) and β-caryophyllene (≤0.47%). The
compounds commonly presented in oxygenated derivative subgroup,
including alcohols (α-terpineol, linalool, geraniol, etc., ≤6.75%), alde­
hydes (geranial, neral, etc., ≤2.96%), esters (geranyl acetate, neryl ac­
etate and octyl acetate, ≤0.81%), oxides (limonene oxide and linalool
oxide, ≤0.90%) and other chemicals (nootkatone, ≤2.54%). The struc­
tures of these compounds and their levels in pomelo peel essential oils
were summarized in Fig. 1 and Supplementary material 5, respectively.
3.1.2. Sensory notes of pomelo peel essential oils
It must be noted that the contribution of each compound to the
fragrance of pomelo peel essential oils not only depend on its concen­
tration. Alternatively, the contribution of each constituent in a blend of
odorants is usually estimated according to its odor activity value
(Cheong, Liu, et al., 2011). It is defined as the ratio of constituent con­
centration in the blend to its odor threshold As for pomelo peel essential
oils, although monoterpenes were the richest constituents, they
contributed to aroma perception in a less extent due to their higher
threshold values. In contrast, the oxygenated compounds presented in
medium levels, but their lower thresholds made them be major con­
tributors in the fragrance of pomelo peel essential oils. Consequently,
aldehydes, terpene alcohols and nootkatone were identified as potent
odorants in pomelo peel essential oils (Cheong, Loke, Liu, Pramudya, &
Yu, 2011). From fractal geometry, the aldehydes such as neral and
geranial gave a fresh lemony note, while terpene alcohols including
linalool, 4-terpineol, citronellol, farnesol, nerolidol, nerol and geraniol
substantially contributed to floral, tea-like and woody notes. For the
odor features of other aroma-active compounds, the details could be
founded in a previous reference (Cheong, Liu, et al., 2011) and the
sensorial perception parameters of the monomers in pomelo peel
essential oils were summarized in Supplementary material 6.
3.1.3. Bioactivities of pomelo peel essential oils
Besides its attractive fragrance, numerous studies had been carried
on the potential bioactivities of pomelo peel essential oils. The results
definitively declared its diverse bioactivities including antimicrobial,
antioxidant and anti-melanogenic activities. A wide antimicrobial
spectrum was evidenced for pomelo peel essential oils, which displayed
effective inhibitions against Penicillium chrysogenum, Bacillus subtilis,
Staphylococcus aureus, Escherichia coli, Salmonella paratyphi B, Listeria
monocytogenes, Candida albicans, Aspergillus flavus, Streptococcus iniae,
Mucor hiemalis, Penicillium expansum and Fusarium proliferatum (Guo

Table 1
The relative percentages (%) of structure-grouped chemicals in the essential oils from pomelo peels.
Material Monoterpenes Sesquiterpenes Alcohol Aldehyde Ester Oxide Nootkatone Ref

Peel 92.20 1.80 0.00 0.73 0.00 0.00 ud1 He et al. (2019)
Peel 94.40 0.60 1.00 0.30 0.00 0.90 ud Chen et al. (2018)
Peel 88.92 1.24 0.40 0.63 0.00 0.00 0.13 Sawamura, Kuwahara, Shichiri, and Aoki (1990)
Peel 98.44 0.33 0.31 1.09 0.00 0.18 0.12
Peel 87.31 0.89 3.43 0.47 0.00 0.00 0.04
Peel 95.45 0.47 0.58 0.59 0.00 0.00 0.06
Peel 90.08 1.58 0.32 0.32 0.00 0.00 0.06
Peel 97.13 1.33 0.32 0.31 0.00 0.05 0.14
Peel 94.77 1.07 0.24 0.18 0.00 0.10 0.95
Peel 98.69 0.30 0.37 0.14 0.00 0.07 0.30
Peel 93.21 0.21 0.44 1.12 0.60 0.00 1.07 Zhou, Zhou, Jiang, and Xie (2006)
Peel 84.14 0.90 6.75 0.54 0.61 0.00 1.75
Peel 84.68 2.09 0.00 0.13 0.00 0.00 ud Shao et al. (2015)
Peel 89.90 0.38 0.00 2.04 0.00 0.00 ud
Peel 96.33 1.44 0.00 0.00 0.00 0.00 ud
Peel 91.32 0.00 0.00 0.00 0.00 0.00 ud
Peel 96.05 0.00 0.79 2.81 0.00 0.35 ud Dang et al. (2016)
Peel 79.60 0.00 0.00 2.00 0.00 0.00 ud Ndiaye et al. (2017)
Peel 97.07 0.00 0.26 0.38 0.00 0.00 ud Lan-Phi and Vy (2015)
Peel 98.93 0.00 0.00 0.00 0.00 0.00 ud
Peel 98.26 0.92 0.00 0.00 0.00 0.00 ud
Peel 99.54 0.00 0.00 0.08 0.00 0.00 ud
Peel 98.55 0.56 0.08 0.21 0.00 0.00 ud
Peel 97.37 0.21 0.00 0.00 0.00 0.00 1.27 Saviuc, Dascălu, Chifiriuc, Rădulescu, and Lazăr (2010)
Peel 93.25 0.09 1.64 0.52 0.09 0.39 1.92 Chaiyana et al. (2014)
Peel 92.04 0.23 0.10 1.50 0.21 0.50 nd2
Peel 89.52 0.26 1.93 2.96 0.08 0.61 2.54
Peel 87.25 0.50 0.82 0.88 0.14 0.32 1.34
Flavedo 83.76 0.57 0.33 0.70 0.16 0.08 0.35 Sawamura, Shichiri, Ootani, and Zheng (1991)
Flavedo 82.19 0.67 0.38 0.50 0.04 0.01 0.28
Flavedo 79.88 0.47 0.52 1.06 0.02 0.03 0.03
Flavedo 78.19 1.43 0.31 1.09 0.03 0.19 0.16
Flavedo 83.83 1.04 0.49 0.55 0.18 0.07 0.46
Flavedo 80.92 0.04 0.31 0.07 0.28 0.01 0.36
Flavedo 78.66 0.45 0.82 0.88 0.24 0.00 0.10
Flavedo 85.25 0.44 0.47 1.05 0.14 0.00 0.07
Flavedo 97.50 0.33 0.30 0.80 0.00 0.30 0.10 Njoroge, Koaze, Karanja, and Sawamura (2005)
Flavedo 95.51 0.65 0.59 0.58 0.81 0.00 0.59 Tao and Liu (2012)
Flavedo 98.40 0.23 0.20 0.30 0.00 0.00 tr3 Tu et al. (2002)
1
ud refers to undetectable;
2
nd refers to not detected;
3
tr refers to trace.

3
L. Xiao et al.
Fig. 1. The structures of the compounds in pomelo peel essential oils.
et al., 2018; Lan-Phi & Vy, 2015; Tao & Liu, 2012; Van Hung, Chi, & Phi,
2013). The corresponding minimum inhibitory concentrations (MIC) of
Escherichia coli, Pseudomonas aeruginosa, Salmonella paratyphi B, Listeria
monocytogenes, Staphylococcus aureus, Bacillus subtilis, Candida albicans
and Aspergillus flavus were determined as 5 μL/mL, 80 μL/mL, 5 μL/mL,
40 μL/mL, 2.5 μL/mL, 5 μL/mL, 2.5 μL/mL and 1.25 μL/mL, respectively
(Guo et al., 2018). It must be noted that different MIC values were re­
ported for Penicillium chrysogenum (4.69 μL/mL), Bacillus subtilis (9.38
μL/mL), Staphylococcus aureus (9.38 μL/mL) and Escherichia coli (37.50
4
Food Chemistry 351 (2021) 129247
μL/mL) (Tao & Liu, 2012). These inconsistencies possibly derived from
the differences in applied pomelo variety. The antimicrobial activity of
pomelo peel essential oils was mainly ascribed to its terpenes, aldehydes
and alcohol constituents, such as ocimene, β-myrcene, α-pinene,
β-pinene, ρ-cymene, α-phellandrene, β-phellandrene, β-caryophyllene,
citral, citronellal, linalool, 4-terpineol and α-terpineol. The possible
underlying working mechanism of these constituents included attacking
the phospholipid bilayer of cellular membrane, disrupting enzyme sys­
tems, damaging genetic substances and forming fatty acid
L. Xiao et al.
hydroperoxidase induced by the oxygenation of unsaturated fatty acids,
inhibiting bacteria growth (Burt, 2004; Chen, Lin, Lin, & Jen, 2018).
Generally, in contrast to bacteria, mould and yeast displayed higher
susceptibilities to pomelo peel essential oils. Due to the stronger hy­
drophilic nature of outer membrane, Gram-negative bacteria were often
less sensitive to pomelo peel essential oils than Gram-positive bacteria
(Diao, Hu, Feng, Li, & Xu, 2013; Trombetta et al., 2005). In vitro ex­
periments to scavenge ABTS and DPPH radicals, the half maximal
inhibitory concentrations (IC50) of peel essential oils from various
pomelo varieties were determined at the range of 43.8 mg/mL ~ 63.1
mg/mL (Lan-Phi & Vy, 2015). The in vivo anti-melanogenic activities of
pomelo peel essential oils were tested with B16 melanoma cells, in
which the essential oils at a concentration higher than 10 μg/mL
significantly decreased melanin content in a dosage-dependent manner
(He, Li, Peng, He, & Pan, 2019). It was achieved by inhibiting tyrosinase
expression to block melanin synthesis pathway, in which tyrosinase
catalyzes the key steps of melanogenesis.
3.1.4. Extraction of pomelo peel essential oils
Obviously, the above-mentioned pleasant odor and bioactivities
constructed solid foundations for the potential utilization of pomelo peel
essential oils in food, cosmetics and pharmaceutical industries. How­
ever, the efficient production of pomelo peel essential oils is the first as
well as the most crucial factor deciding the feasibility of its large-scale
application. Traditionally, cold pressing, steam distillation, hydro­
distillation, solvent extraction and simultaneous distillation-solvent
extraction were the most common regimes employed in recovering
essential oils from pomelo peels. Regardless of their recovery rates, these
regimes were time-consuming and their batch operations usually took
over 2 h. Besides, the involvement of organic solvents in solvent
extraction and simultaneous distillation-solvent extraction made it
environmentally unfriendly (Lucchesi, Chemat, & Smadja, 2004). To
this end, a solvent-free microwave extraction (SFME) was developed, in
which the pomelo peels was distilled by microwave heating without
adding solvents or water. The results showed that SFME operated for 30
min at 150 W and 300 W gave essential oils yields of 0.19 mL/100 g and
0.21 mL/100 g, respectively. These values were higher than that of 3-h
hydrodistillation (0.17 mL/100 g). In comparing with 4-h hydro­
distillation, the microwave assisted extraction (MAE) for 24 min pre­
sented the comparable yield rate (1.88%/1.91%), higher oxygenation
fraction (48.59%/29.63%) as well as lower energy consumption (0.15
kW h/1.54 kW h) and environmental impact (123.20 g CO2/1232 g CO2)
(Liu, Zu, & Yang, 2017). In terms of total volatile concentration in ob­
tained products, the methods were arranged in an order of 4-h cold
pressing (0.78 g/mL), 100 ◦ C-2 h hydrodistillation (0.76 g/mL), 500 W-
50 s microwave-assisted solvent extraction (0.72 g/mL), 10-min
ultrasonic-assisted solvent extraction (0.67 g/mL) and 40 ◦ C-15 MPa
supercritical fluid extraction (0.45 g/mL). In short, the above-mentioned
novel regimes were promising in fabricating higher-quality pomelo peel
essential oils in a more sustainable way (Vongsangnak, Gua, Chau­
vatcharin, & Zhong, 2004).
Besides its technical performance, the recovery regimes exerted great
impacts on the chemical composition of pomelo peel essential oils, thus
altering its odor characteristics and bioactivities (Sun, Ni, Yang, Chen
et al., 2014; Phi, Hung, Chi, & Dung, 2015). The effects of various re­
covery regimes on the sensory description and chemical composition of
pomelo peel essential oils were summarized in Table 2 and Supple­
mentary material 7. Obviously, both sensory description and chemical
composition highly relied on recovery methods. In contrast to hydro­
distillation, microwave-assisted extraction could produce an essential
oils presenting a natural pomelo odour (Liu et al., 2017). Similarly, the
pomelo peel essential oils obtained by vacuum-distillation exhibited
lower antioxidant and antimicrobial activities than that by cold-pressing
(Phi et al., 2015). Solvent extraction (ethyl acetate) was more effective
than hydrodistillation in producing a pomelo peel essential oils against
Saccharomyces cerevisiae and Aspergillus fumigatus (Chanthaphon,
5
Food Chemistry 351 (2021) 129247
Chanthachum, & Hongpattarakere, 2008). The pomelo peel essential
oils from supercritical fluid extraction (MIC = 2.5 µL/mL) were better
than those from vacuum-distillation and cold-pressing (MIC > 2.5 µL/
mL) in inhibiting Staphylococcus aureus and Candida albicans (Thava­
napong, Wetwitayaklung, & Charoenteeraboon, 2010). Obviously, the
method-induced variation in chemical composition triggered the
method-dependent nature of the sensory perception and bioactivity of
pomelo peel essential oils. Firstly, the dissolving-out or evaporating
rates of pomelo peel constituents were method specific. Secondly, the
derivatization of extracted constituents as well as their inter-conversions
generally occurred and substantially changed from method to method
(Li et al., 2016). For example, the exposure to oxygen at 70 ◦ C signifi­
cantly increased the levels of limonene oxides and L-carvone in pomelo
peel essential oils, thus resulting in stronger sweet, floral and minty
notes (Sun et al., 2018). Similarly, an oily off-flavor was perceived in
sunlight-exposed pomelo peel essential oils (Sun, Ni, Yang, Wu et al.,
2014). Based on these observations, it was highly recommended that
frequency-oriented or bioactivity-oriented regimes should be developed
instead of the traditional yield-oriented one.
3.1.5. Application of pomelo peel essential oils
The pleasant aroma and diverse bioactivities of pomelo peel essential
oils provide a solid base for its application in foods, cosmetics and
pharmaceuticals. A novel natural food preservative was formulated by
mixing an emulsion of pomelo peel essential oils (0.4%) with a chitosan
solution (0.03%) (Chen et al., 2018). It was found that its antimicrobial
capacity for inhibiting E. coli was highly improved by decreasing the size
of emulsion droplets via homogenization, probably due to the improved
capacity of the oil to permeate the hydrophilic pericellular membrane
(Moghimi, Ghaderi, Rafati, Aliahmadi, & McClements, 2016). In addi­
tion, the emulsified pomelo peel essential oils presented a higher anti­
oxidant capacity than its free counterpart in terms of DPPH radical
scavenging capacity and linoleic peroxidation inhibition (Chaiyana,
Phongpradist, & Leelapornpisid, 2014). In non-surgical endodontic
retreatment, pomelo peel essential oil was a better solvent than orange
oils and xylene in softening old gutta-percha filling from root canal prior
to its removal (Surapipongpuntr, Chaisomboon, & Piyapattamin, 2014).
3.2. Pectin from pomelo peels
3.2.1. Structural characters of pomelo peel pectin
Structurally, pectin has a backbone composed by D-galacturonic acid
(GalA) units via α-(1 → 4) linkage, which randomly interrupted by L-
rhamnose (Rha) residues with side chains of D-galactose (Gal) and L-
arabinose (Ara). Usually, a notable proportion of galacturonic acid units
in pectin is methylated. However, the degree of esterification of pectin
(DE, the percentage of the carboxyl groups methylated) is origin spe­
cific. Based on DE, pectin can be categorized into low-methoxyl (LM, DE
< 50) and high-methoxyl (HM, DE > 50) pectin. In describing the
structure of a pectin, DE, molecular weight and GalA content often
presented, ranging from 1.7% to 91.83%, from 0.13 × 105 Da to 6.45 ×
105 Da and from 10.46% to 95.5%, respectively. Moreover, the
monosaccharide-based parameters of branching density (Rha/GalA,
0.01 ~ 0.12), side chain length [(Ara + Gal)/Rha, 1.65 ~ 22.83],
linearity [GalA/(Fuc + Rha + Ara + Gal + Xyl), 2.44 ~ 8.40], HG
fraction (GalA-Rha, 56.89% ~ 88.69%) and RG-I fraction (2Rha + Ara
+ Gal, 11.20% ~ 40.31%) were applied in pomelo peels. These
monosaccharide-based parameters of pomelo peel pectin were similar to
that of Citrus peel pectin, while slightly lower than the figure for apple
pectin (Mao et al., 2019; Wikiera, Mika, Starzynska-Janiszewska, &
Stodolak, 2015).
3.2.2. Rheological behaviors of pomelo peel pectin
It is well-known that rheological properties of pectin dispersion are
related to its molecular structures (Qin et al., 2017; Willats, Knox, &
Mikkelsen, 2006). In contrast to citrus and apple pectin, the rheological
 L. Xiao et al.
Table 2
The yield, characteristic odours and composition of essential oils from pomelo peels based on different extraction methods.
Material Extraction Key extraction conditions Yield Composition (relative percentage, %) Ref
regime
Monoterpenes Sesquiterpenes Alcohols Aldehydes Esters Oxides Others

Fresh peel HD Sample/water = 1/10 (g/mL), 4 h 0.24% (w/w, Chanthaphon et al.

wb) (2008)
Fresh peel SE Ethyl acetate, solid/liquid = 1/4 (g/mL), 8 h 1.57% (w/w,
wb)
Fresh peel CP Water, centrifugation 3000 rpm for 10 min 1.16% (v/w, wb) 99 0.1 0.2 0.2 0.1 0 0 Thavanapong et al.
Fresh peel VSD 65 ◦ C, − 600 bar, 3 h 2.39% (v/w, wb) 98.9 1.5 0.2 0.2 0 0 0 (2010)
Dry peel SFE Carbon dioxide, 13 MPa, 40 ◦ C, 3 h 0.4% (v/w, wb) 97.1 0.4 0.5 0.4 0.2 0 0.1
Dry peel HD Sample/citric acid solution (0%~0.55%) = 1/ 4.58 ~ 4.68% 92.92 ~ 94.89 0.05 ~ 0.07 0.24 ~ 0.06 ~ 0.1 0.04 ~ 0.16 ~ 0 Tuan et al. (2019)
3 (g/mL), 2.5 h (w/w, db) 0.32 0.05 0.30
Dry peel HD Sample/water = 1/6 (g/mL), 3 h 0.17 mL/100 g 86.84 0.52 0.27 0.87 0.46 0 4.8 Chen et al. (2016)
Fresh peel MD Microwave power 150 ~ 450 W, 1.5 h 0.19 ~ 0.21 mL/ 80.98 ~ 92.43 0.45 ~ 0.62 0.73 ~ 0.047 ~ 0.41 ~ 0 3.86 ~
100 g 1.31 0.25 0.66 9.28
Fresh CP Brine, centrifugation 4000 g for 15 min 0.03% (w/w, 85.83 0 0.04 0 0 0 0 Phi et al. (2015)
flavedo wb)
Fresh VSD 70 ◦ C, 0.7 bar, 3.5 h 0.04% (w/w, 86.24 0 0 0 0 0 0
flavedo wb)
6

Fresh HD Sample/water-1/4 (g/mL), 4 h 1.91% (v/w, db) 55.16 2.51 4.05 1.03 0 0.56 13.91 Liu et al. (2017)
flavedo
Fresh MD Microwave power 230 ~ 700 W, 30 ~ 24 min 1.5 ~ 1.95% (v/ 32.63 2.04 5.09 0.7 0 0.86 24.02
flavedo w, db)
Fresh CP Icy brine, centrifugation at 13,500g for 5 min 5.4 mg/g (wb) 95.31 1.17 0.4 2.71 0.07 0.03 0.02 Li et al. (2016)
flavedo
Fresh CP Icy brine, centrifugation at 13,500g for 5 min 1.15% (w/w, 94.62 2.04 0.83 1.92 0.1 0.01 0.06 Sun, Ni, Yang, Chen et al.
flavedo wb) (2014)
Fresh HD Sample/water = 1/2 (g/mL), 2 h 2.55% (w/w, 91.28 1.2 3.49 1.23 0.09 0.1 1.92
flavedo wb)
Fresh SDE Sample/water = 1/10 (g/mL), sample/n- 1.79% (w/w, 90.7 1.67 1.84 1.84 0.12 3.25 0.07
flavedo hexane = 1/3 (g/mL), 2 h wb)
Fresh M− SE n-Hexane, microwave power 500 W, 50 s 2.02 (w/w, wb) 94.52 0.49 1.27 1.95 0.11 0.03 1.26
flavedo
Fresh U-SE n-Hexane, ultrasonic power 35 kHz, 10 min 1.90 (w/w, wb) 94.06 0.63 1.25 2.12 0.1 0.03 1.36
flavedo
Fresh SFE Carbon dioxide, 15 MPa, 40 C, centrifugation
◦
4.13 (w/w, wb) 87.48 2.93 2.94 0.58 0.21 0.93 3.58
flavedo at 13,500 g for 5 min

Food Chemistry 351 (2021) 129247

*HD: hydrodistillation; SE: solvent extraction; CP: cold pressing; VSD: vacuum steam distillation; SFE: supercritical fluid extraction; MD: microwave distillation; SDE: simultaneous distillation and extraction; M− SE:
microwave-assisted solvent extraction; U-SE: ultrasonic-assisted solvent extraction; TVC: Total volatile chemicals.
L. Xiao et al.
properties of pomelo peel pectin were not elaborately explored and no
more than ten articles had been published on this point. As for high
methoxy pomelo pectin (DE = 58%; Mw = 353 kDa), its dispersion
behaved as a Newtonian liquid at a concentration below 0.6% (w/v) and
a pseudoplastic liquid at a concentration above 0.6% (w/v) (Gamo­
npilas, Krongsin, Methacanon, & Goh, 2015). In temperature sweep
tests, the dispersion at 0.4% (w/v) showed liquid-like characteristic in
the tested temperature range (10 ◦ C ~ 50 ◦ C). In the concentration range
of 0.6% ~ 0.8% (w/v), the dispersion was liquid-like at high tempera­
ture and gel-like at low temperature, respectively. As the concentration
reached 1% w/v, the dispersion was gel-like among the studied tem­
perature range. Regrettably, the data on the intrinsic rheological prop­
erties of low methoxy pomelo pectin were unavailable and it was often
reported in the presence of sugar or calcium ion.
As for the gelation behavior and gel properties, the high methoxy
pomelo pectin itself usually underwent gelation at a concentration
above 1.0% (w/v) and resulted in weak gels. However, its critical
gelation concentration sharply decreased or the gel strength signifi­
cantly increased in the presence of sufficient acid (pH 2 ~ 3), sugar
(50% ~ 60%, w/w) and divalent ions (Ba2+, Ca2+, Mg2+). The high
methoxy pomelo pectin demonstrated better gelling properties than the
commercial citrus pectin with similar DE and MW in terms of gel
modulus and yield stress (Gamonpilas et al., 2015; Qin et al., 2017). In
contrast, the presence of divalent ion (Ca2+) was essential for the gela­
tion of low methoxy pomelo pectin (DE = 41%) (Norziah, Kong, Abd
Karim, & Seow, 2001). Regardless of its DE, the gels from pomelo pectin
exhibited a pseudoplastic behaviour with shear thinning characteristic
(n < 1). Importantly, the pseudoplastic property of polysaccharide sys­
tems certainly benefited liquid foods to be pumped more easily and
obtain a thinner consistency with better mouth feel (Vardhanabhuti &
Ikeda, 2006).
3.2.3. Extraction of pomelo peel pectin
Pectin shows great potential as a functional ingredient in food and
pharmaceutical applications due to its valuable gelling, stabilizing and
thickening properties. However, pectin exists as a cell wall adhesive to
work by crosslinking other biopolymers. Furthermore, pectin matrix is
embedded within the single networks of cellulose microfibril, hemicel­
lulose or protein as well as their hybrid networks, which made
extracting pectin quite difficult (Panouillé, Thibault, & Bonnin, 2006).
Due to this fact, a lower yield (≤14.5%) was often concluded by using
hot water to extract pectin from pomelo peels (Table 3). In improving
extraction efficiency, the pectin extraction was generally assisted by
chemical adjuvants or physical techniques. The latter mainly referred to
microwave, ultrasound, high-speed shear and even their combinations.
In general, these assistance decomposed the polymeric networks,
liberated pectin and hemi-cellulosic materials that intrinsically attached
to cellulose microfibrils, polysaccharides and lignins, thus improved
pectin extractability (Bergmans, Beldman, Gruppen, & Voragen, 1996).
The reported extraction regimes and their yields and impacts on the
physicochemical characters of obtained pomelo peel pectin were sum­
marized in Table 3.
Obviously, chemical-assisted extraction has been widely developed
as the mainstream technology to recovery pomelo peel pectin. The re­
ported pectin yields ranged from 3.11% to 39.72% and highly depended
on the material, the chemical adjuvant and its concentration, the oper­
ating parameters such as the solid/solvent ratio, extraction time, tem­
perature and precipitant. Usually, dried peel, flavedo and albedo were
used as starting material and the fresh peel was used rarely. Regarding
the chemical nature of adjuvants, they could be grouped into mineral
acid, organic acid, alkaline and ion liquid. The mineral acid group
mainly consisted of HCl, HNO3 and NaHSO4, while the application cases
of citric acid, tartaric acid, oxalic acid, ethylenediamine-tetraacetic acid
and lactic acid were evidenced in organic acid group. The alkaline
adjuvant normally referred to caustic soda (NaOH), while [HO3S
(CH2)4mim]HSO4 and [Bmim]Cl were reported as ionic liquid adjuvants
7
Food Chemistry 351 (2021) 129247
in extracting pomelo peel pectin. Among of them, the acid adjuvant was
the most popular and only one investigation had been reported with
alkaline adjuvant.
It must be noted that the working way and extracting efficiency are
adjuvant specific. The acid adjuvants favored the release of pectin by
disrupting the internal networks and bonding of pomelo peels due to the
attack of glycosidic bonds by H3O+. This was verified by the fact that,
with pomelo albedo as material, the boiling water extraction gave pectin
yields between 9.96% and 14.44% (w/w) and the further ammonium
oxalate-assisted extraction with the resultant residual gave a second
pectin yield ranging from 7.19% to 10.77% (w/w). As for alkaline ad­
juvants, the presented hydroxyl ions solubilized the polymeric networks
of pomelo peels by destroying the intermolecular hydrogen bonds of
polysaccharides and the ester bonds of polysaccharide-lignin (Bergmans
et al., 1996). Regarding the acid and alkaline concentration, an optimal
value was reported to achieve the maximum pectin yield. For acid-
assisted extraction, most cases evidenced that pectin yield increased
with pH decrease, while a few exceptions reported the yield decrease at
extremely low pH, such as below 1.6 (Table 3). For alkaline-assisted
extraction, a parabolic function was concluded for the pH dependence
of pectin yield, which often peaked around pH 12.6 (Wandee, Uttapap,
& Mischnick, 2018). The yield decrease in extreme pH values were
ascribed to pectin degradation induced by acid or alkaline (Wandee
et al., 2018). As for ionic liquid adjuvants, they were not applied alone as
acids or alkali did. In fact, they have been used as a secondary adjuvant
in microwave-acid-assisted extraction to further improve pectin yield
(Liu, Qiao, Gu, et al., 2017). In this case, an optimal dosage of ionic
liquid (10 mmol/L for [HO3S(CH2)4mim] HSO4) was evidenced in
considering the fact that the elevated viscosity by high levels of ionic
liquid suppressed the pectin release (Liu, Qiao, Yang, Gu, & Yang, 2017).
Besides the product yield, chemical adjuvants exerted non-ignorable
effects on the structures and size of the obtained pectin molecules. In
terms of degree of esterification (DE), the value with acid adjuvants
ranged from 53.9% to 92.75% and generally increased with acid con­
centration, which certainly implied the acquisition of high methoxyl
pomelo peel pectin (HM, DE > 50%). For example, DE value increased
from 53.9% to 82.5% by increasing HCl concentration from 25 mM to
200 mM. This was due to the convert of non-methylesterified carboxyl
groups into methyl-esterified carboxyl groups during acid extraction
(Wandee et al., 2018). It must be noted that exceptional cases were also
reported. The results of Methacanon, Krongsin, and Gamonpilas (2014)
showed that acid extraction (HCl or HNO3) at pH 2 gave lower DE values
(64.1% and 59.4%) than that at pH 3 (70.7% and 62.5%) (Methacanon
et al., 2014). On the other hand, pomelo peel pectin from alkaline-
assisted extraction was often characterized as low methoxyl pectin
(DE < 50%) due to the saponification reaction of non-methylesterified
carboxyl groups in the presence of alkaline. As reported, the DE value
declined from 1.7% to 0.0% as alkaline concentration increased from 25
mM to 50 mM (Wandee et al., 2018). Similar to alkaline-assisted
extraction, only one report was available for subcritical water extrac­
tion and the results implied that low methoxyl pomelo pectin (DE =
40.1%) was obtained when the extraction performed at 30 bar, 120 ◦ C
for 140 min (Liew, Teoh, Tan, Yusoff, & Ngoh, 2018). The low DE was
interpreted as a consequence of the prolonged exposure to high pressure.
In terms of the average molecular weight (Mw) of pomelo pectin, the
figures treated with alkaline adjuvant ranged from 1.42 × 105 Da to
1.87 × 105 Da, lower than that with acid adjuvant (1.71 × 105 Da ~
3.56 × 105 Da) (Wandee et al., 2018). The lower Mw was probably due to
the co-occurrence of depolymerization and demethylation of pomelo
pectin in alkaline environment (Wandee et al., 2018).
Obviously, the chemical-assisted extractions were superior to hot
water extraction in product yield and property modulation. However,
the time- and energy-consuming disadvantages of hot water extraction
persisted in the chemical-assisted extractions and, furthermore, they
were often criticized for their environmental threats resulted from using
excessive chemicals. To this end, novel methods were proposed by
L. Xiao et al. Food Chemistry 351 (2021) 129247

Table 3
The yields and physicochemical properties of pomelo peel pectin obtained by different extraction methods.
Material Method Extracting conditions (solvent, solid/liquid, Yield % (w/ DE (%) c Mw (×105 GalA (%) e Ref.
a b
temperature, time, (assistance), precipitant) w, db) Da) d

Fresh CAE Citric acid (0 ~ 0.55%), 1/3, boiling, acid CaCl2 11.0 ~ 24.0 Tuan et al. (2019)
peel (2 N)
Oil-free CAE HCl (pH 2.0), 1/18, 90 ◦ C, 90 min, ethanol 3.11 Chen et al. (2016)
peel
CMAE HCl (pH 1.5), 1/18, 5.6 min, (M 520 W), ethanol 3.29
Dry peel CAE HCl (pH 2.2), 1/8, 75 ◦ C, 1 h, ethanol 19.0 39.2 73.9 Norziah, Fang, and Karim
CAE Citric acid (pH 4.0), 1/8, 75 ◦ C, 1 h, acetone 20.8 40.5 74.9 (2000)
CAE NaHSO4 (1%, pH 2.2), 1/8, 75 ◦ C, 1 h, 1.75% (v/ 12.6 40.3 39.9
v) Al2(SO4)3 + 1.05% (v/v) Na2CO3
Dry peel CMAE Water, 1/30, 25 ◦ C, 30 min, (M 1100 W, 2 min), 6.5 29.7 0.43 70.0 Wandee et al. (2018)
ethanol
CMAE HCl (pH 2.5/1.6/1.4/1.0), 1/30, 25 ◦ C, 30 min, 12.1/20.5/ 53.9/71.2/ 1.71/3.27/ 84.4/85.0/
(M 1100 W, 2 min), ethanol 17.1/16.1 79.3/82.5 3.68/3.56 83.8/82.2
CMAE NaOH (pH 11.7/12.1/12.6/13.0), 1/30, 25 ◦ C, 30 13.9/24.2/ 1.7/-/-/- 1.87/1.42/ 83.9/85.7/
min, (M 1100 W, 2 min), ethanol 22.0/19.4 1.52/1.69 83.6/80.9
Dry peel CMAE Tartaric acid (0.25% w/v, pH 1.5), 1/40, 30 ◦ C, 23.83 92.75 Quoc et al. (2015)
9.0 min, (M 660 W), ethanol
Dry peel CMAE Oxalic acid (0.25% w/v, pH 4.22), 1/36.05, 30 ◦ C, 18.58 91.83 Quoc, Anh, Tien, and Trang
8.5 min, (M 660 W), ethanol (2014)
Dry peel CMAE Ethylenediamine-tetraacetic acid (0.25% w/v, pH 38.38 79.1 3.49 70.74 You et al. (2019)
1), 1/25, 125 s, (M 550 W), ethanol
CUAE Ethylenediamine-tetraacetic acid (0.27% w/v, pH 31.37 72.59 2.89 86.49
0.5), 1/25, 70 ◦ C, 81 min, (U 900 W), ethanol
Dry peel CAE Citric acid (pH 1.8), 1/29, 88 ◦ C, 2.34 h, ethanol 39.72 57.56 0.91 68.54 Qin et al. (2017)
CAE Lactic acid/glucose/water (15/5/3 w/w/v, pH 23.04
0.56), 1/29, 50 ◦ C 1 h, ethanol
Dry peel HWE Water, 1/29, 88 ◦ C, 2.34 h, ethanol 5.34 36.65 Liew, Teoh, Yusoff, and Ngoh
CUMAE Water, 1/29, (U 40 kHz, 27.5 min; M 643 W, 6.40 3.68 39.37 (2019)
min), ethanol
Dry peel CMAE Citric acid (pH 1.8), 1/29, 6.40 min, (M, 643.44 27.65 64.11 – 48 Liew et al. (2016)
W), ethanol
CUAE Citric acid (pH 1.8), 1/29, 27.52 min, (U 40 kHz), 14.25 64.4 – 10.46
ethanol
CMUAE Citric acid (pH 1.8), 1/29, (M 643.44 W, 6.40 min 30.5 67.01 – 74.92
→ U 40 kHz, 27.52 min), ethanol
CUMAE Citric acid (pH 1.8), 1/29, (U 40 kHz, 27.52 min 36.33 59.85 0.93 71.09
→ M 643.44 W, 6.40 min), ethanol
Dry peel SWE Subcritical water (30 bar), 1/10, 120 ◦ C, 61 min, 19.6 40.1 0.63 76.62 Liew et al. (2018)
ethanol
Dry peel CAE HCl (pH 1.24), 1/50, 85 ◦ C 1.5 h, ethanol 17.5 76.6 1.52 Guo et al. (2017)
CHSAE HCl (pH 1.24), 1/50, 240 s, (high-speed shearing), 20.9 74.4 1.91
ethanol
Dry HWE Water, 1/25, boiling, 1 h, ethanol 5.18 ~ 9.29 69.32 ~ 0.21 ~ 0.38 68.31 ~ Chaidedgumjorn et al. (2009)
flavedo 72.13 72.58
Dry HWE Water, 1/25, boiling 1 h, ethanol 9.96 ~ 74.99 ~ 0.41 ~ 0.50 74.27 ~ Chaidedgumjorn et al. (2009)
albedo 14.44 78.21 79.29
Dry CAE HCl (pH 2/3) with 1.6 mM CaCl2, 1/30, 80 ◦ C, 2 h, 19.33/11.06 64.1/70.7 6.45/5.62 86.26/72.81 Methacanon et al. (2014)
albedo ethanol
CAE HNO3 (pH 2/3) with 1.6 mM CaCl2, 1/30, 80 ◦ C, 2 24.26/8.32 59.4/62.5 4.4/4.82
h, ethanol
Dry CAE HCl (pH 2.5), 1/10, 80 ◦ C 1 h, ethanol/methanol/ 4.94/ 8.97/ -/92.12/- -/95.5/- Vega, Jaraba, Perez, Arrieta,
albedo 1-propanol 3.85 and Quinones (2018)
Dry CAE HCl (pH 2.5), 1/26, 100 ◦ C, 3 h, ethanol 18.97 64.9 Liu et al. (2017)
albedo
CMAE [HO3S(CH2)4mim] HSO4 (10 mM)/HCl (pH 2.5), 29.16/25.88
1/26, 100 ◦ C, 15 min, (M 331 W), ethanol
Dry CAE HCl (pH 2.5), 1/27, boiling, 3 h, ethanol 19.72 Liu et al. (2017)
albedo
CMAE [Bmim]Cl (1.0 M), 1/23, 15 min, (M 385 W 10 21.04
min), ethanol
CUMAE [HO3S(CH2)4mim]HSO4 (10 mM)/HCl (pH 2.5), 32.86/26.93 -/62.4
1/27, 15 min (U 40 kHz + M 36 0 W), ethanol
a
HWE: hot water extraction; CAE: chemical-assisted extraction; CMAE: chemical- and microwave-assisted extraction; CUAE: chemical- and ultrasound-assisted
extraction; CMUAE: chemical-, microwave-, and ultrasound-assisted extraction; CUMAE: chemical-, ultrasound- and microwave-assisted extraction; CHSAE: chemi­
cal and high-speed shearing-assisted extraction; SWE: subcritical water extraction.
b
Solid/liquid was expressed in w/v; U and M refer to ultrasound and microwave assistance, respectively; → means a sequential assistance, while + means
simultaneous assistance.
c
DE is the degree of esterification.
d
Mw is molecular weight.
e
GalA is galacturonic acid.

8
L. Xiao et al.
applying certain physical means to assist the chemical-assisted extrac­
tion regimes. The primarily methods included microwave, ultrasound,
high-speed shear and the combination of microwave and ultrasound.
Like acid and alkaline adjuvants, these means facilitated pectin release
from cell wall by degrading the involved polymeric networks but they
worked in diverse way. For microwave, it could rapidly heat and
evaporate the moisture, sharply increase the pressure in cells and thus
rupture plant tissue and cell walls as a consequence of steam explosion
(Dhobi, Mandal, & Hemalatha, 2009). For ultrasound, the damage to
polymeric networks or cell wall was attributed to its cavitations, which
was interpreted well in elsewhere (Liew, Ngoh, Yusoff, & Teoh, 2016).
In terms of high-speed shear, the polymeric networks or cell walls were
pulled apart or crashed by the powerful shearing force and fierce particle
collisions (Guo et al., 2017). It must be noted that both microwave and
ultrasound not only disrupt the intrinsic integrality of plant tissues or
cell walls but also lead to the degradation of solubilized biopolymers at
an enough high intensity. Thus, in terms of product yield, an optimal
intensity (power, time or their combination) should be executed, and the
insufficient and the excessive intensity should be avoided. However, the
optimal operating intensity of microwave- and ultrasound-assistance
was case specific and should be determined individually. In fact,
microwave-assistance was much popular than ultrasound-assistance in
extracting pomelo peel pectin. Although they were not of strict
comparability, the available cases indicated that the microwave-
assistance improved product yield by 0.18% ~ 23.78%, while these
values were not available for sole ultrasound-assistance. For the com­
bination of microwave and ultrasound, two assistance models were
applied, namely, first microwave then ultrasound (M → U) or first ul­
trasound then microwave (U → M). On the basis of microwave-
assistance, the combined assistance resulted in increases in product
yield by 8.68–11.82% and U → M was better than M → U.
In contrast to chemical-assistances, physical technique-assistances
often led to minor changes in the molecular structure of extracted
pomelo peel pectin. Only a tiny variation in DE value (59.85% ~
67.01%) was observed among the pomelo peel pectin obtained with
various physical technique-assistances, narrower than that with
chemical-assistances (≤92.75%) (Liew et al., 2016). It must be noted
that physical technique-assistances bring about significant changes in
the molecular weight of pomelo peel pectin, especially when they are
operated at higher power or extended duration. For example, the in­
crease in microwave power from 550 W to 770 W was accompanied with
the decrease in Mw from 1.32 × 105 Da to 0.76 × 105 Da and extension of
microwave time from 5 min to 15 min led to the decrease in Mw from
1.32 × 105 Da to 0.77 × 105 Da (Wandee et al., 2018). In comparison,
the chemical-assistances were more effective than the physical
technique-assistances in improving pectin yield and tuning its physico­
chemical properties. Thus, in practice, the physical technique-
assistances were seldom applied alone and, alternatively, they were
often operated with chemical adjuvant-assistances in efficiently recov­
ering pomelo pectin. The pros and cons of above-mentioned extraction
regimes were summarized in Supplementary material 8.
3.2.4. Applications of pomelo peel pectin
Pectin had been widely used as a thickener, stabilizer or emulsifier in
food, pharmaceutical and chemical industries due to its valuable gelling,
stabilizing and thickening properties. In food industry, upon 90-d stor­
age, carrot jam with pomelo peel pectin demonstrated comparable ca­
pacities to that with commercial pectin in retaining ascorbic acid, total
phenol and β-carotene, but the former showed a better color stability
(Roy et al., 2017). Pomelo peel pectin could substantially improve the
performance of the edible packaging film based on chicken feather
protein in moisture absorption (13.83%), water solubility (95.5%),
breakage strength (285.89 g) and elongation (13.17%) (Das, Borah, &
Badwaik, 2017). The resultant film could protect fried fish fillet from
weight loss, texture hardening and bacteria spoilage upon 5-d storage. In
contrast to the untreated samples, fresh strawberries coated with pomelo
9
Food Chemistry 351 (2021) 129247
pectin/sodium alginate demonstrated lower values in water loss, decay
and malondialdehyde content while higher values in soluble protein,
soluble solid, vitamin C and superoxide dismutase (SOD) activity (Chen
& Zeng, 2017). Interestingly, the incorporation of pomelo peel pectin
(12 wt% on wheat flour basis) could significantly lower the calories
(31.44 kcal) of instant noodles and thus imparted it with better efficacy
in weight control (Jitpukdeebodintra & Jangwang, 2009). In pharma­
ceutical industry, the microparticles (2 μm ~ 5 μm) made from pomelo
peel calcium pectinate via the ionotropic gelation showed excellent
ibuprofen encapsulation (the ibuprofen-to-pectin ratios ranging from
1:10 to 1:50) and thus improved its solubility (43% ~ 74%) in pH 7.5
phosphate buffer (Sriamornsak, Konthong, & Nunthanid, 2012). More­
over, pomelo peel pectin was used as a stabilizer to assist the synthesis of
cerium oxide nanoparticles (≤40 nm) and the resultant nanoparticles
(4.0 mg/mL) were free from cytotoxicity and displayed an excellent 2,2-
diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity
(73.36%) as well as the strong antimicrobial activities against E. coli and
B. subtilis. (Patil, Paradeshi, Chaudhari, Mishra, & Chaudhari, 2016). In
chemical industry, the pomelo peel pectin was successfully used as a
novel natural kinetic hydrate inhibitor for methane upon the subcooling
up to 12.5 ◦ C by blocking the growth of methane hydrate crystals and
thus facilitated the pipeline transportation of methane in oil and gas
industries (Xu et al., 2016).
3.3. Polyphenols from pomelo peels
3.3.1. Major constituents in pomelo peels polyphenols
Polyphenols are the main phytochemical components with signifi­
cant antioxidant, anti-inflammatory, antimicrobial, anti-nervous disor­
der and anti-metabolic disorder activities. As shown in Supplementary
material 3, pomelo peels possessed rich polyphenols at a range of
1799.04 mg/100 g ~ 5364.00 mg/100 g. The structure-grouped
chemicals of pomelo polyphenols mainly included flavonoids and
phenolic acids (Supplementary material 9). The flavonoids could be
classified into three groups, namely, flavonones (24.56 mg/100 g wb ~
1320.00 mg/100 g wb), flavones (≤18.20 mg/100 g wb) and falvonols
(≤16.60 mg/100 g wb). Flavonones were mainly consisted of naringin
(1270.00 mg/100 g wb ~ 23.90 mg/100 g wb), naringenin (≤56.01 mg/
100 g wb), narirutin (≤22.00 mg/100 g wb), hesperidin (≤9.44 mg/100
g wb), neohesperidin (≤7.65 mg/100 g wb), eriocitrin (≤4.76 mg/100 g
wb), hesperetin (≤0.56 mg/100 g wb) and eriodictyol. Flavones were
comprised of rhoifolin (≤14.0 mg/100 g wb), tangeretin (≤4.6 mg/100
g wb), neodiosmin (≤3.5 mg/100 g wb), nobiletin (≤3.48 mg/100 g
wb), diosmin (≤0.7 mg/100 g wb) and sinensetin (≤0.3 mg/100 g wb).
Flavonol primarily referred to rutin (≤0.18 mg/100 g db). Additionally,
phenolic acids were constituted by gallic acid, chlorogenic acid, ferulic
acid, caffeic acid, sinapic acid and coumaric acid. The levels and
structures of these pomelo polyphenols were summarized in Supple­
mentary material 10 and 11, respectively.
In different parts of peels, flavedo was richer in most flavonoids and
phenolic acids in compared with albedo. Detailedly, pomelo flavedo had
the high levels of hesperetin (≤67.55 mg/100 g db), eriocitrin (≤17.14
mg/100 g db), hesperidin (≤14.23 mg/100 g db), naringenin (10.18
mg/100 g db ~ 62.25 mg/100 g db), nobiletin (≤6.24 mg/100 g db),
tangeretin (≤5.19 mg/100 g db), sinensetin (≤3.42 mg/100 g db) and
eriodictyol (0.83 mg/100 g db ~ 6.09 mg/100 g db), while pomelo al­
bedo was rich in naringin (≤1400 mg/100 g wb), diosmin (≤95.79 mg/
100 g db) and flavonol (4.47 mg/100 g db ~ 19.33 mg/100 g db).
Flavedo was also high in gallic acid (52.70 mg/100 g db ~ 109.66 mg/
100 g db) in contrast to albedo (6.61 mg/100 g db ~ 40.76 mg/100 g
db).
3.3.2. Bioactivities of pomelo peels polyphenols
Till now, the pomelo peel polyphenols were evidenced with antiox­
idant, anti-inflammatory, antimicrobial and anti-nervous disorder and
anti-metabolic disorder activities. For antioxidant activity, the pomelo
L. Xiao et al.
polyphenol acted as an electron or hydrogen donor to scavenge free
radicals and reactive oxygen species, thereby preventing many chronic
diseases (Oboh & Ademosun, 2012; Salah et al., 1995). Usually, pomelo
peel polyphenols work in a dose-dependent manner in scavenging
DPPH, 2,2-azinobis-3-ethylbenzthiazoline-6-sulphonate (ABTS),
hydrogen and superoxide anion radicals as well as in reducing ferric ions
(FRAP). In DPPH assay, pomelo peel polyphenol extracts showed IC50
values in the range of 40.0–122.06 μg/mL (Fidrianny, Sari, & Ruslan,
2016). However, an IC50 value up to 22.3 mg/mL was concluded by Lim
and Loh (2016), who uncovered that the polyphenol extracts from
pomelo peels was inferior to that from other citrus peels (IC50, 7.51 mg/
mL ~ 12.91 mg/mL) in DPPH radical scavenging capacity. The discor­
dances among different researches might result from different materials
and extraction methods applied, which ultimately changed the purity
and composition of resultant polyphenol extracts. It was worthy to
mention that the antioxidant activity of polyphenols heavily depended
on their structures. For instance, the flavonoid compound with hydroxyl
configuration often presented strong hydroxyl, peroxyl, and peroxyni­
trite radical scavenging capacities (Heim, Tagliaferro, & Bobilya, 2002).
The flavonoid aglycones showed a higher antioxidant activity than
flavonoid glycosides. More information about structure–activity re­
lationships of flavonoids was minutely analyzed by Heim et al. (2002).
The anti-inflammatory activity of pomelo peel polyphenols was
probably attributed to their down-regulation capacities for
inflammation-related genes and proteins (Wang et al., 2017). For lipo­
polysaccharide treated PC12 cells, naringin (200 ng/mL ~ 1000 ng/mL)
from pomelo peels successfully decreased the levels of inflammation-
related proteins in a dose-dependent manner (Wang et al., 2017). In
mice, the pomelo peel polyphenol extracts (300 mg/kg ~ 500 mg/kg)
displayed considerable inhibitions (34.47% ~ 38.68%) against the
carrageenan-induced paw edema, although these values were signifi­
cantly lower than that of ibuprofen (76.31%) (Ibrahim et al., 2018). The
anti-inflammatory activity of pomelo peel polyphenols was ascribed to
cut back the release of amino alkane and 5-hydroxytryptamine, which
triggered the inflammatory process (Ibrahim et al., 2018).
The protective effects of pomelo peel polyphenols on neurodegen­
erative disorders attracted much attentions recently. These effects
resulted from the inhibition of neurological disorder-related cell
apoptosis by pomelo peel polyphenols. For lipopolysaccharide-induced
PC12 cells, the treatment of pomelo peel naringin (200 ng/mL, 600
ng/mL and 1000 ng/mL) significantly improved cell survival (61.2%,
73.1% and 87.36%) in a time- and concentration-dependent manner
(Wang et al., 2017). In mechanism, naringin firstly downregulated cy­
tochrome P450 2E1, inhibited the release of reactive oxygen species,
mitigated the stimulation of oxidative stress and rectified the antioxi­
dant protein contents. Secondly, naringin lowered inflammation-related
genes and protein expression. Finally, naringin markedly attenuated the
cytochrome c by shifting from the mitochondria to the cytosol and
regulated caspase-3-related protein expression. For APPswe/PS1dE9
transgenic mouse model of Alzheimer’s disease, naringin (100 mg/kg/
day) improved long-term cognitive function via increasing CaMKII
(calcium/calmodulin-dependent protein kinase II) activity by the
phosphorylation at Thr286 (Wang et al., 2013).
For the antimicrobial activity of pomelo peel polyphenols, the fla­
vonoids fraction showed a wide antimicrobial spectrum against Escher­
ichia coli, Pseudomonas aeruginosa, Bacillus subtilis, Staphylococcus aureus,
Chromobacterium violaceum and Vibrio anguillarum with the minimum
inhibitory concentrations (MIC) of 4.5 mg REs/mL, 0.5 mg REs/mL, 3.5
mg REs/mL, 0.5 mg REs/mL, 3.0 mg REs/mL and 3.0 mg REs/mL,
respectively (Liu, Pan, Li, Jie, & Zeng, 2017). The flavonoids could
penetrate the hydrophobic region of lipid bilayer by interacting with
phospholipids of cell membrane to damage bacteria cell membrane
permeability, accompanied with cell constituents release, metabolic
dysfunction and the inhibition of protein synthesis, finally leading to cell
pyknosis and death (He, Wu, Pan, & Xu, 2014; Yao et al., 2012).
Besides the above-mentioned bioactivities, the phenolic extracts of
10
Food Chemistry 351 (2021) 129247
pomelo peels were capable of preventing metabolic disorders, including
diabetes mellitus, hyperlipidemia, hypertension, obesity, fatty liver and
insulin resistance (Caengprasath, Ngamukote, Maekynen, & Adi­
sakwattana, 2013; Ding et al., 2013; Oboh & Ademosun, 2011). The
anti-hyperglycemia of pomelo peel polyphenols was derived from the
following ways. Firstly, the pomelo peel polyphenols were found with
α-amylase and α-glucosidase inhibiting activities and the slowing-down
effects on the conversion of starch to glucose, thereby moderating the
postprandial blood glucose (Bischoff, 1994; Kwon, Vattem, & Shetty,
2006). The inhibiting capacities of pomelo peel polyphenols to sugar
lyases were dose-dependent but the working manners of free and bound
phenolics were somewhat different (Lim & Loh, 2016). In terms of
α-amylase inhibiting rate, the bound phenolics (12.91% ~ 64.24%) was
consistently higher than the free phenolics (2.08% ~ 25.22%) in tested
concentration range (Lim & Loh, 2016). In terms of α-glucosidase
inhibiting rate, the free phenolics (74.45%) was better than the bound
(45.99%) at a low concentration (<80.0 mg/mL) while they were
comparable in the high concentration range (160.0 mg/mL ~ 320.0 mg/
mL). Secondly, the anti-hyperglycemia of pomelo peel polyphenols was
related to their improvements in insulin resistance. For high-fat diet-fed
C57BL/6 mice, the administration of pomelo peel polyphenol extracts
for 8-weeks successfully blocked the body weight gain, lowered fasting
blood glucose, improved glucose tolerance and insulin resistance and
lowered serum insulin levels (Ding et al., 2013). The improvements of
pomelo peel polyphenols on glucose intolerance and insulin resistance
were attributed to the up-regulated transcription of GLUT4 and the
elevation of PPARα (Ding et al., 2013). The former is the insulin-
regulated glucose transporter and the latter is a ligand-activated tran­
scription factor regulating the glucose metabolism, adipocyte differen­
tiation and lipogenesis. Finally, the pomelo peel polyphenol extracts
were found to restrain the non-enzyme-related protein glycation, limit
the formation of advanced glycation end products, and thus benefit the
prevention of diabetic complications (Caengprasath et al., 2013). As for
the anti-hypertension activity of pomelo peel polyphenol extracts, a
dose-dependent manner was concluded and they inhibited the activity
of angiotensin I-converting enzyme and the transfer of angiotensin I into
angiotensin II (Ahnfelt-Ronne, 1991).
3.3.3. Extraction of pomelo peel polyphenols
To use pomelo peel polyphenols as an additive, its extraction effi­
ciency is of extreme importance. Traditionally, the pomelo peel poly­
phenols were extracted by using various solvents, including water,
organic solvent, mineral acid, alkali, ion liquid and carbon dioxide.
Obviously, for a specific starting material, the extracting performance
differed among solvents due to their distinguished solubilizing capac­
ities to pomelo peel polyphenols (Yang et al., 2011). The high solubi­
lizing capacity meant a strong diffusion rate of polyphenols, which
accelerated the target compounds to transfer from pomelo peels to sol­
vent. Not only the product yield, but also the chemical composition of
pomelo peel polyphenols depended on the applied solvent. Among
common solvents, the organic solvents were better than water to gain
the extract with high total phenolic content (TPC). For example, the TPC
(22.0 mg GAE/g db) in the methanolic extract of pomelo peels was
higher than that in the water extract (Tsai, Chang, & Chang, 2007). In a
three-stage sequential extraction process of pomelo peel polyphenols by
n-hexane, ethyl acetate and ethanol, the TPC values were concluded as
26.2 mg GAE/g db, 37.8 mg GAE/g db and 68.8 mg GAE/g db,
respectively (Fidrianny et al., 2016). Besides this, the TPC value would
vary with the solvent concentration. For example with ethanol, the
maximum total flavonoid content was found with ethanol concentration
at 80% ~ 90% and it decreased as ethanol concentration either
increased or decreased. To extract bound phenolics, the solid residue
from free phenolics extraction was subjected to alkaline or acid hydro­
lysis, in which inner network of pomelo peels as well as the linkages
between phenolics and cell wall materials were destroyed, thereby
releasing the bound one. For instance, the free phenolics in pomelo peels
L. Xiao et al. Food Chemistry 351 (2021) 129247

was extracted by 80% aqueous acetone and then the bound phenolics
was obtained by ethyl acetate extraction after NaOH treatment, with
TPC values of the extracts at 6.5 mg GAE/g db and 3.4 mg GAE/g db,
respectively.
Besides the solvent applied, the extraction efficiency with organic
solvents relied on the material process and the operating parameters
such as the solid/solvent ratio, extraction time and temperature and
precipitant. Usually, dried pomelo peels were applied for recovering
phenolics, while there was only one report that used fresh peels. For the
material process, its drying history played an important role in
extracting phenolics. In comparison, the ethanol extract from the dried
pomelo albedo by oven drying (50 ◦ C/60 ◦ C, 24 h) gave higher total
flavonoid contents (13.30 mg GAE/g db/13.37 mg GAE/g db) than that
by freeze drying (12.68 mg GAE/g db) (Rahman, Shamsudin, Ismail,
Shah, & Varith, 2018). This was attributed to the heat-induced release of
bound phenolics (Rahman et al., 2018). The effects of extraction
methods on the extraction efficiency and properties of pomelo poly­
phenols were shown in Table 4. Clearly, traditional solvent extraction
was the most popular regime to recovery polyphenols from pomelo
peels. Additionally, it is difficult to compare the results from different
researches because they evaluated the extraction efficiency in different
ways like phenolics, flavonoid or naringin yields.
To further improve the extraction efficiency, the physical assistances
were suggested to couple with the solvent extraction. The physical

Table 4
The extraction efficiency and properties of polyphenols from pomelo peels based on different extraction methods.
Materials Methoda Brief description of the method Extraction efficiencyb Extracts propertiesc Ref.

Dried peel CSE Water/methanol, S/L 1/100, room TPC: -/22.0 mg GAE/g db S-DPPH‧: 20% of vitamin C and butylated Tsai et al. (2007)
temperature, 24 h hydroxytoluene
Dried peel CSE Methanol (80%), 1/20, 30 ◦ C, 3 h TPC: 3.01 ~ 4.07 mg GAE/ FRAP: 0.65 ~ 1.01 mM Fe2+/100 g FW; RP: 1.14 Toh, Khoo, and Azrina
g FW; TFC: 2.29 ~ 3.57 mg ~ 1.49 mM TE/100 g wb (2013)
QE/g wb
Dried peel CSE Hot water, S/L 3/20, 4 h, Naringin yield: 1.12/ Sudto et al. (2010)
-/dichloromethane 0.44%
CSE Water, S/L 1/6, 70 ◦ C → methanol, S/ Naringin yield: 0.59 →
L 3/50; 30 min 2.4/%
Dried peel CSE Methanol, S/L 1/10, 25 ◦ C, 24 h Phenolic yield: 24.34% S-DPPH‧: IC50 22.30 mg/mL; FRAP: 141.25 mM Lim and Loh (2016)
Fe2+/g db
CSE Acetone (80%) → ethyl acetate, S/L Phenolic yield: 13.72 → α-Amylase inhibitory activity: 38.17%→38.04%;
1/10, 25 ◦ C, 10 min 32.43%; TPC: 89.8 → α-Glucosidase inhibitory activity: 41.06%→
15.92 mg GAE/g db 30.26%
Dried peel CSE n-Hexane → ethyl acetate → ethanol TPC: 26.2 → 37.8 → 68.8 S-DPPH‧: IC50 122.06 → 35.0 → 44.96 μg/mL Fidrianny et al. (2016)
mg GAE/g db; TFC: 33.1 →
56.9 → 11.7 mg QE/g db
Dried peel CSE Acetone (80%) → ethyl acetate, S/L TPC: 6.5 → 3.4 mg GAE/g S- DPPH‧: EC50 1.6 → 1.9 mg/mL; S-OH‧: EC50 5.6 Oboh and Ademosun (2012)
1/5 db; TFC: 0.31 → 0.40 mg → 16.1 mg/mL; Fe2+ Chelating ability: 0.71 →
GAE/g db 1.3 mg/mL; Inhibition to Fe2+-induced lipid
peroxidation: 156.1 → 142.8 μg/mL
Dried peel CSE Acetone (80%) → ethyl acetate TPC: 6.5 → 3.4 mg GAE/g Oboh and Ademosun (2011)
db
Dried peel CSE Ca(OH)2 (0.1%), S/L 1/16, 100 ◦ C, TFC: 135 mg RE/g db Jiang et al. (2014)
1.5 h
CSE-MR Ca(OH)2 (0.1%), S/L 1/16, 100 ◦ C, TFC: 105.6/ 807.4/ 587.4/
1.5 h, resin ethanol (0/30/50/70/ 682.7/ 431.1 mg RE/g db
90%)
Dried peel UAE Ethanol (80%), S/L 1/38, 40 kHz, TFC: 7.26 mg RE/g db High antioxidative activity. Jiang et al. (2014)
56 ◦ C, 1.75 h
Dried peel UAE- Ethanol (70%), S/L 2/15, 40 kHz, 30 Naringin yield: 2.2%; The Tang, Zhu, Zhong, and Zhou
MR min purification of naringin: (2011)
77.26%
Dried peel CSE Ethanol (85%), S/L 1/15, 80 ◦ C, 45 Flavonoids yeild: 1.51% S-OH‧:31.1 ~ 71.3%; S-O2‧: 18.1 ~ 61.3%; S- Ru et al. (2013)
min DPPH‧: 32.1 ~ 69.3%; FRAP: 3212.4 µM Fe2+/g
MAE Ethanol (85%), S/L 1/15, 1000 W, Flavonoids yield: 2.32% S-OH‧:35.2 ~ 80.4%; S-O2‧: 27.2 ~ 70.4%; S-
80 ◦ C, 45 min DPPH‧: 35.2 ~ 80.5%; FRAP: 4734.6 µM Fe2+/g
SFE Carbon dioxide, S/L 1/15, 40 MPa, Flavonoids yield: 2.37% S-OH‧:40.5 ~ 84.4%; S-O2‧: 30.5 ~ 78.4%; S-
80 ◦ C, 45 min DPPH‧: 48.5 ~ 89.4%; FRAP: 5690.6 µM Fe2+/g
Dried CSE fresh-/freeze-/oven-dried, ethanol TFC: 11.60/10.45/ S-DPPH‧: 45.82/86.21/87.92–85.03%; FRAP: Rahman et al. (2018)
flavedo (80%), S/L 1/20, 30 ◦ C, 3 h 12.26–11.67 mg GAE/ g db -/4/2.61–3.69 mM Fe2+/g db
Dried CSE fresh-/freeze-/oven-dried, ethanol TFC: 18.76/12.68/ S-DPPH‧: 22.85/93.03/92.25–89.26%; FRAP:
albedo (80%), S/L 1/20, 30 ◦ C, 3 h 13.3–13.37 mg GAE/ g db 3.69/2.45/4.34–3.80 mM Fe2+/g db
Dried CSE Ethanol (95%), S/L 1/10, 80 ◦ C, 30 TPC: 2.16 mg GAE/g db S-DPPH‧: 70.14%; FRAP: 12.27 mg TE/mL db Pichaiyongvongdee,
flavedo min Rattanapun, and Haruenkit
Dried CSE Ethanol (95%), S/L 1/10, 80 ◦ C, 30 TPC: 2.72 mg GAE/g db S-DPPH‧: 66.07%; FRAP: 15.68 mg TE/mL db (2014)
albedo min
Dried CSE HCl (pH 2.5), S/L 1/26, 100 ◦ C, 3 h Naringin yield: 6.78 mg/g Liu et al. (2017)
albedo MAE Water/ [HO3S(CH2)4min] HSO4 (10 Naringin yield: 4.99/8.38/
mmol/L)/HCl (pH 2.5)/ Na2SO4(10 4.83/4.32 mg/g
mmol/L), S/L 1/26, 331 W, 15 min
a
CSE: conventional solvent extraction; UAE: ultrasound assisted extraction; UAE-MR: ultrasound assisted extraction conbined with macroporous resin purification
technology; SFE: supercritical fluid extraction; MAE: microwave assisted extraction; S/L: solid/liquid expressed in w/v; U and M refer to ultrasound and microwave
assistance, respectively; → means a sequential assistance, while + means simultaneous assistance;
b
TPC: total phenolic contents; TFC: total flavonoid content; GAE: gallic acid equivalent; QE: quercetin equivalent; RE: rutin equivalent; TE: trolox equivalent; DPPH:
2,2-diphenyl-1-picrylhydrazyl; ABTS: 2,2′ -azinobis-3-ethylbenzthiazoline-6-sulphonate; FRAP: ferric reducing antioxidant power
c
S-DPPH: the scavenging ability to DPPH radical. S-OH‧: the scavenging ability to hydroxyl radical. S-O2‧: the scavenging ability to superoxide anion radical. FRAP:
ferric reducing antioxidant power. IC50: 50% inhibiting concentration. EC50: concentration for 50% of maximal effect.

11
L. Xiao et al.
measures involved microwave, ultrasound and their combinations and
they worked in similar ways as described in the part of pomelo peel
pectin extraction. For example, the microwave-assistance could increase
the flavonoids yield of ethanol extraction by 0.81% (Ru, Cai, & He,
2013). For ultrasound-assisted ethanol extraction, the highest total
flavonoid content (7.26 mg RE/g db) was achieved for the extract as the
extraction was operated with a solid/liquid ratio of 1/38 g/mL for 1.75 h
at 56 ◦ C in 80% aqueous ethanol. The decrease in total flavonoid content
upon the excessive extension of ultrasound-assistance (>1.75 h) was
probably due to the oxidization of flavonoids (Jiang, Shen et al., 2014).
Moreover, [HO3S(CH2)4mim]HSO4 (10 mM) as an ion liquid adjuvant
sharply improved naringin yield (4.99 → 8.38 mg/g) based on
microwave-assisted water extraction (Liu, Qiao, Yang, et al., 2017).
The extraction regime not only affected the product yield of poly­
phenols from pomelo peels, but also changed the chemical composition
of the product, thus regulating its physicochemical properties and bio­
activities. For example, in terms of solvent, pomelo peel polyphenol
extracts were in a TPC order of ethanol (6.88%) > ethyl acetate (3.10%)
> n-hexane (2.62%), while in an IC50 order of ethanol (122.06 μg/mL)
> n-hexane (44.96 μg/mL) > ethyl acetate (35.0 μg/mL) in scavenging
DPPH radicals (Fidrianny et al., 2016). It suggested that the product
yield, chemical composition and bioactive performance should be
addressed simultaneously when extract pomelo peel polyphenols. In this
case, the extraction regime and operating parameters should be
designed in a product functionality-oriented manner. For instance,
methanol extraction combined with dichloromethane crystallization
obtained high-purity naringin with a yield at 2.4% (Sudto, Pornpakakul,
& Wanichwecharungruang, 2010).
3.3.4. Application of pomelo peels polyphenols
The applications of pomelo peel polyphenols mainly based on their
bioactivities. In considering its antimicrobial activity, the flavonoid
extract from pomelo peels was incorporated into chitosan-based food
packaging film to protect bread from mold and prolong the shelf life of
bread (16-day/with vs 8-day/without) (Sugumaran et al., 2017). Upon
14-day storage, the chicken wing treated with ethyl acetate extract of
pomelo peels (0.1% ~ 1%) presented a lower total viable count, a lower
2-thiobarbituric acid value and a higher sensory score than the un­
treated counterpart (Klangpetch, Phromsurin, Hannarong, Wichaphon,
& Rungchang, 2016). For postharvest mango, the treatment with the
ethanol extract of pomelo albedo substantially suppressed the mango
anthracnose pathogen (Colletotrichum gloeosporioides) about mycelial
growth (37.47% ~ 39.75%↓) and spore germination (53.98% ~
62.86%↓) (Naradisorn, 2015). In view of its antioxidant capacity, the
ethanol extract from pomelo peels was used as a natural antioxidant for
lard and its efficacy at 0.8% w/w was comparable to the synthetic
antioxidant butylated hydroxytoluene at 0.02% w/w (Ding, Su, Xu, &
Jing, 2000). Similarly, the flavonoids concentrate from pomelo peels
successfully inhibited the lipid peroxidation of fish tissue (Zarina & Tan,
2013). In pharmaceutical industry, the hot-water extract from pomelo
peels (600 mg/kg) could reduce the worm burden, ova count and
oogram in Schistosoma mansoni infected mice via significantly improving
IgM and IgG antibody (Ahmed, Bahnasy, & Zedan, 2015). Interestingly,
the ethyl acetate extract from pomelo peels (≥10 mg/L) could be uti­
lized as a repellent to completely prevent oviposition capacity of gravid
female Aedes aegypti mosquito, thereby controlling its population and
disease transmission (Malar, Jamil, Hashim, Kiong, & Jaal, 2017). In oil
and gas industries, the ethanol extract of pomelo peels was used as a
corrosion inhibitor for N80 steel (Sun et al., 2017). In 3.5% NaCl solu­
tion saturated with CO2, the presence of the extract (0.4 g/L) could
decrease the corrosion rate from 2.49 mg cm− 2h− 1 to 0.35 mg cm− 2h− 1.
The inhibition action was ascribed to forming an adsorption film of
polyphenol molecules on the metal surface, hindering the metal disso­
lution (Ahamad & Quraishi, 2010; ji, Shukla, Dwivedi, Sundaram, &
Prakash, 2011).
12
Food Chemistry 351 (2021) 129247
3.4. Other components
Besides the above-mentioned components, there were other bioac­
tive compounds existing in pomelo peels although they were in lower
levels, such as coumarins, furanocoumarins, bioactive polysaccharides,
limonins and carotenoids. Coumarins are a group of secondary metab­
olites in citrus plants, while furanocoumarins constitute a subclass of
coumarins with an additional furan ring linked at the C6/C7 or C7/C8
position (Bourgaud et al., 2006). The coumarins presented in pomelo
peels around 154.59 mg/100 g db (Supplementary material 3),
approximately including 54 monomers (structures shown in Supple­
mentary material 12) and demonstrating diverse bioactivities such as
anti-inflammatory, antioxidant, hepatoprotective and neuroprotective
activities. For anti-inflammatory activity, the xylene-induced ear edema
of mice could be significantly suppressed by auraptene (2 mg/kg) iso­
auraptene (0.5 mg/kg), and meranzin hydrate (3 mg/kg) with inhibition
ratios of 26.2%, 35.6% and 19.5%, respectively, while marmin showed
less inhibitory effects on the auricle swelling at 1 mg/kg and 0.5 mg/kg
(Zhao, Yang et al., 2019). Additionally, the low doses of auraptene,
isoauraptene, meranzin hydrate and marmin (<3 mg/kg) displayed
excellent suppressing effects against carrageenan-induced subacute
inflammation in mice, with inhibition ratio between 28.3% and 44.1%
(Zhao, Yang et al., 2019). The anti-inflammatory action of pomelo
coumarins had achieved by suppressing the lipopolysaccharide-induced
secretion of inflammatory cytokines, such as IL-1β, PGE2 and TNF-α. For
hepatoprotective activity, columbianoside II (49.0%), meranzin hydrate
I (36.5%), meranzin hydrate II (42.6%) and bergaptol (32.6%) were
superior to bicyclol (positive control, 16.2%) in the inhibition rate of D-
galactosamine-induced LO2 cell apoptosis at a dose of 20 μM (Tian et al.,
2019). The hepatoprotective effects of pomelo coumarins was ascribed
to their regulating capacities for the cellular antioxidant pathway. As a
result, the D-galactosamine-induced decreases in GSH-Px and SOD ac­
tivities and the main members of antioxidant defense system in cells
were inhibited. Moreover, auraptene, a major coumarin in pomelo peels,
could increase the bile flow and biliary bile acid output, suppress bile
acid synthesis and inhibit the hepatic uptake of bile acids, thus allevi­
ating 17α-ethinylestradiol-induced cholestasis (Tian et al., 2019). For
neuroprotective activity, pomelo peel auraptene was able to activate
ERK1/2 and CREB in cultured neurons and PC12 cells and to induce the
neurite outgrowth from PC12 cells (Furukawa, Watanabe, Okuyama, &
Nakajima, 2012).
From a structure view, the water-soluble polysaccharides in pomelo
peels were referred to pectin analogues, which were composed by
galactose, rhamnose, xylose, glucose, glucuronic acid, galacturonic acid
and arabinose. They presented comparable Mw values (1.10 × 105 Da ~
4.60 × 105 Da) to above-mentioned pectin (Wu et al., 2020; Yu, Ji, &
Liu, 2018). Compared to the polysaccharides from other pomelo tissues,
the one from pomelo peels demonstrated the stronger scavenging ca­
pacities to DPPH and OH radicals and the higher inhibiting efficacy to
HeLa cells (Wu et al., 2020). In tumor-bearing mice, the bioactive
polysaccharides from pomelo peels were capable of inducing the
apoptosis of solid tumor cells through its immunity enhancing effect (Yu
et al., 2018).
As for limonins, they widely presented in pomelo peels around 4.7
mg/g and were regarded as the major compounds for the undesirable
bitter taste of citrus juice (Yang et al., 2017). In β-carotene bleaching
assay, the antioxidant capacity of limonins from pomelo flavedo was
higher than that of Vc but lower than that of limonins from Citrus
reticulata and Citrus changshanensis (Sun, Chen, Chen, & Chen, 2005).
Regarding the pomelo peel carotenoids, it varied from 1.68 mg/100 g to
69.5 mg/100 g in various pomelo species and demonstrated consider­
able scavenging capacities to ABTS and DPPH radicals (Yoo & Moon,
2016).
L. Xiao et al. Food Chemistry 351 (2021) 129247

4. Conversion of pomelo peels into adsorbents, biofuels and Table 5

others Application of pomelo peel in pollutants adsorption (heavy metals, dyes, oils and
others).
4.1. Adsorbents Adsorbents Pollutant Qma Ref.

Heavy metal
Due to the abundant functional groups including hydroxyl, carbonyl, Pomelo peel power Pb2+ 2.14 Yu and He (2018)
carboxyl, phenolic and ether moieties, pomelo peels had been widely Pomelo peel power Cd2+ 21.83 Saikaew and
utilized as an adsorbent in its original or modified form for wastewater Kaewsarn (2011)
Pomelo peel power Cr6+ 0.57 Wang et al. (2020)
treatment (Sud, Mahajan, & Kaur, 2008). The pomelo peel-based
FeCl3-modified pomelo peel Cr6+ 21.55
adsorbent functioned via combining with target objects by different power
inter-molecular forces such as electronic exchange, electrostatic inter­ Pomelo peel power Cu2+ 19.7 Tasaso (2014)
action, ion exchange, hydrogen bonding, precipitation, complexation Depectinated pomelo peel Cu2+ 21.1
and reduction (Inyang et al., 2016; Nguyen et al., 2020; Zheng, Sun, Li, power
Pomelo peel power UO2+ 31.28 Yang et al. (2019)
& Du, 2020). The combination efficiency relied on the adsorbent nature Isopropyl azodicarboxylic
2
UO2+ 42.73
2
(porous structures, surface areas, functional groups, etc.), object acid-modified starch-
(charge, hydrophobicity, hydrophilicity, functional groups, etc.) and pomelo peel pulp
adsorption conditions (pH, temperature, ion strength, etc.). As reported, Pomelo peel K2FeO4-activated Cr6+ 209.64 Yin et al. (2019)
biochar
the pomelo peel absorbents could be used to eliminate pollutants such as
Pomelo peel H3PO4-activated Cr6+ 57.64 Wu et al. (2017)
heavy metals, dyes and oils from wastewater (Table 5). The aimed heavy biochar
metals included Pb2+, Cd2+, Cr6+, Cu2+, UO2+ 2 , Ag , Mn
+ 2+
and Tl+. The Pomelo peel H3PO4-activated Ag+ 127.1 Zhao, Ying et al.
intended dyes comprised of methyl orange, malachite green, methylene biochar Pb2+ 86.76 (2018)
blue, reactive blue 114, methyl red, congo red, reactive red 21 and acid Pomelo peel NaOH-activated Mn2+ 163.19 An, Miao, Zhao, Li,
biochar and Zhu (2020)
blue 15. Diesel, lubricating oil, soya bean oil, crude oil and pumpkin
Pomelo peel biochar Tl+ 4.28 Gao et al. (2020)
seed oil could also be adsorbed by pomelo peel absorbents. Pomelo peel H3PO4-activated Cr6+ 57.64 Tao, Wu, and Cha
To improve the performance of original pomelo peel absorbent, it biochar (2019)
was often subjected to carbonization, physical and chemical modifica­ Polyetherimide-grafted and Cu2+ 74.2 Tang et al. (2020)
FeCl3-modified pomelo peel
tions, which imparted the original absorbent with more adsorption sites
power
and/or new functional groups (Wang, Zhou, Kuang, Jiang, & Yang,
2020). For carbonization, the original pomelo peels were processed at Dye
Pomelo peel H3PO4-activated Methyl orange 165.02 Tao et al. (2019)
high temperature (250 ◦ C ~ 800 ◦ C) in an inert atmosphere to make a
biochar
porous biochar (Wu et al., 2017; Zhao, Ying et al., 2018). For chemical Polyetherimide-grafted and Malachite 530 Tang et al. (2020)
modification, some chemical modifiers were often incorporated into FeCl3-modified pomelo peel green
pomelo peel powder before carbonization to improve the adsorbing power
performance of resultant biochar. The common chemical modifiers Pomelo peel power Reactive blue 16.3 Argun, Güclü, and
114 Karatas (2014)
included NaOH, KOH, H3PO4, FeCl3, Fe3O4, K2FeO4 and K2CO3 Pomelo peel power Methylene blue 344.83 Hameed,
(Table 5). These chemicals could activate the biochar by increasing Mahmoud, and
surface pore size, surface area and oxygen-containing groups, thus Ahmad (2008)
enhancing its holding capacity of pollutants (Wang et al., 2020). Occa­ Pomelo peel power Methylene blue 1883.88 Low and Tan
Ultrasound-treated pomelo Methylene blue 7041.52 (2018)
sionally, some chemicals such as isopropyl azodicarboxylic acid, KOH
peel power
and FeCl3 were applied to modify pomelo peel powder without Pomelo peel power Methylene blue 81.71 Ren, Cui, and
carbonization (Yang et al., 2019; Zheng et al., 2020). Moreover, pomelo Citrate-grafted pomelo peel Methylene blue 199.2 Wang (2018)
peels could be chemically modified via grafting reactions with chemicals power
like polyetherimide, polypyrrole, acetic anhydride, amine, citrate, sty­ Pomelo peel KOH-activated Congo red 144.93 Zheng et al. (2020)
power
rene, zirconium oxide and lanthanum hydroxide (Table 5). As a conse­ Pomelo peel K2CO3-activated Methylene blue 222.22 Nowicki,
quence, new functional groups were introduced and attached to pomelo biochar Methyl red 208.33 Kazmierczak-
peels. For physical modification, ultrasound treatment and high shear Razna, and
dispersing were conducted for pomelo peels (Khe & Ching, 2018; Shi Pietrzak (2016)
Pomelo peel KOH-activated Methyl orange 680.2 Li, Sun, Zhang,
et al., 2019). Compared to other regimes such as membrane separation,
biochar et al. (2016)
chemical precipitation and electrochemical treatment, the application of Pomelo peel biochar Reactive red 21 18.59 Nguyen et al.
pomelo peel absorbents was of easier operation, higher efficiency and (2020)
lower cost (Yang et al., 2019; Zhao, Ying et al., 2018). Pomelo peel Fe3O4-activated Reactive red 21 26.25 Foo and Hameed
Besides their applications in wastewater treatment, the pomelo peel biochar Methylene blue 501.10 (2011)
Acid blue 15 444.45
absorbents could be used in other scenarios. Firstly, the original pomelo
peel power was disabled in adsorbing phosphate, while it worked well Oil
Pomelo peel power Diesel 6390 Chai et al. (2015)
with an adsorption capacity of 45.2 mg/g upon the co-modification by
Lubricating oil 9040
ZrCl3 and La hydroxide (Du et al., 2018). Secondly, toward fluoride, Acetic anhydride-grafted Diesel 16,500
polypyrrole-grafted and lanthanum-loaded pomelo peel biochar showed pomelo peel power Lubricating oil 19,390
decent adsorption capacities with 18.52 mg/g and 19.86 mg/g, Styrene-modified pomelo peel Diesel 18,910
respectively (Wang, Chen, Feng, & Li, 2018; Wang, Chen, Li, & Feng, power Lubricating oil 26,360
Pomelo peel-based aerogel/ Soya bean oil 62,600 Shi et al. (2019)
2018). Finally, the pomelo peel biochar with/without chemical modi­
polyvinyl alcohol
fication could adsorb carbamazepine, paracetamol and sulfate at levels Pomelo peel-based aerogel/ Soya bean oil 56,800
of 286.5 mg/g, 286 mg/g and 35.21 mg/g, respectively (Chen, Xie et al., fiber
2017; Tran et al., 2020; Ao, Cao, Hong, Wu, & Wei, 2019). Pomelo peel-based aerogel/ Crude oil 49,200
fiber/ Pumpkin seed 50,500
methyltrimethoxysilane oil
(continued on next page)

13
L. Xiao et al. Food Chemistry 351 (2021) 129247

Table 5 (continued ) was also applied to recovery diversely functional components including
Adsorbents Pollutant Qma Ref. essential oils, pectin, polyphenols, coumarins, etc. Additionally, pomelo
peels as an alternative material to produce adsorbents or biomass fuel
Crude oil 49,800
Soya bean oil 62,300
was developed. These achievements of pomelo peel were due to its
Pomelo peel biochar-based Soybean oil 118.5 Chen, Yu, Shang, excellent physicochemical properties and bioactivities as well as
nanofiber aerogel Han, and Liu advanced biotechnologies. It must be noted that the extraction tech­
(2020) niques could show effects not only on the product yield but also on its
Others
composition, physicochemical properties, bioactivities and structures.
Pomelo peel-based aerogel/ DMSO 51,500 Shi et al. (2019)
fiber/ Chloroform 71,300 Thus, it was highly recommended that functionality- or bioactivity-
methyltrimethoxysilane oriented extraction regimes should be developed in an economic,
Pomelo peel biochar-based Chloroform 120.3 Chen et al. (2020) effective and eco-friendly way. The potentially biological activities and
nanofiber aerogel functional mechanism of these components deserve further discussion.
Amine-crosslinked and Phosphate 53.48 Duan, Xu, Shang,
zirconium oxide-loaded Gao, and Li (2017)
Additionally, more possibilities should be discovered on the application
pomelo peel power of pomelo peels and its functional components in food, pharmaceutical
Dual Zr and La hydroxide- Phosphate 45.2 Du et al. (2018) and chemical industries.
loaded pomelo peel power
Polypyrrole-grafted pomelo Fluoride 18.52 Wang et al. (2018)
peel biochar Declaration of Competing Interest
Lanthanum-loaded pomelo Fluoride 19.86 Wang et al. (2018)
peel biochar The authors declare that they have no known competing financial
Pomelo peel KOH-activated Carbamazepine 286.5 Chen, Xie et al. interests or personal relationships that could have appeared to influence
biochar (2017)
Pomelo peel zirconium oxide- Sulfate 35.21 Ao et al. (2019)
the work reported in this paper.
activated biochar
Pomelo peel biochar Sulfate 1.02 Acknowledgements
Pomelo peel biochar Paracetamol 286 Tran et al. (2020)
a
Qm is the maximum adsorption capacity (mg/g). This work was funded by National Key Research and Development
Program of PR China (2016YFD04002042) and Chongqing Technology
4.2. Ethanol production Innovation and Application Development Key Program (cstc2019jscx-
dxwtBX0031).
The richness in monosaccharide (glucose), disaccharides (fructose,
sucrose), polysaccharides (cellulose, hemicellulose, pectin) and lignin Appendix A. Supplementary data
made pomelo peels suitable for biofuel production. As reported, the
hydrothermally treated (120 ◦ C, 15 min) pomelo peel suspension (15 wt Supplementary data to this article can be found online at https://doi.
%) were sequentially subjected to the saccharification by multienzymes org/10.1016/j.foodchem.2021.129247.
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