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Extraction

This study investigates the extraction of pectin from passion fruit peel using various methods, including acid extraction, ultrasonic-assisted extraction, steam explosion, and a combination of steam explosion with ultrasonic assistance. The results indicate that the ultrasonic-assisted steam explosion method yields the highest pectin extraction with improved emulsion stability and favorable structural properties. The research highlights the potential of utilizing passion fruit peel, a by-product of juice and jam production, for high-quality pectin extraction.

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0% found this document useful (0 votes)
2 views12 pages

Extraction

This study investigates the extraction of pectin from passion fruit peel using various methods, including acid extraction, ultrasonic-assisted extraction, steam explosion, and a combination of steam explosion with ultrasonic assistance. The results indicate that the ultrasonic-assisted steam explosion method yields the highest pectin extraction with improved emulsion stability and favorable structural properties. The research highlights the potential of utilizing passion fruit peel, a by-product of juice and jam production, for high-quality pectin extraction.

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wangjunkai21092k
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foods

Article
Extraction of Pectin from Passion Fruit Peel: Composition,
Structural Characterization and Emulsion Stability
Yonglun Liang 1,† , Yang Yang 1,2,† , Lili Zheng 1,2 , Xiaoyan Zheng 1,2 , Dao Xiao 1,2 , Shenwan Wang 1,2 ,
Binling Ai 1,2 and Zhanwu Sheng 1,2, *

1 Haikou Experimental Station, Chinese Academy of Tropical Agricultural Sciences, Haikou 571101, China
2 Haikou Key Laboratory of Banana Biology, Haikou 571101, China
* Correspondence: [email protected]
† These authors contributed equally to this work.

Abstract: Extraction methods directly affect pectin extraction yield and physicochemical and struc-
tural characteristics. The effects of acid extraction (AE), ultrasonic-assisted acid extraction (UA),
steam explosion pretreatment combined with acid extraction (SEA) and ultrasonic-assisted SEA
(USEA) on the yield, structure, and properties of passion fruit pectin were studied. The pectin
yield of UA was 6.5%, equivalent to that of AE at 60 min (5.3%), but the emulsion stability of UA
pectin was poor. The pectin obtained by USEA improved emulsion stability. Compared with UA,
it had higher protein content (0.62%), rhamnogalacturonan I (18.44%) and lower molecular weight
(0.72 × 105 Da). In addition, SEA and USEA had high pectin extraction yields (9.9% and 10.7%)
and the pectin obtained from them had lower degrees of esterification (59.3% and 68.5%), but poor
thermal stability. The results showed that ultrasonic-assisted steam explosion pretreatment combined
with acid extraction is a high-efficiency and high-yield method. This method obtains pectin with
good emulsifying stability from passion fruit peel.
Citation: Liang, Y.; Yang, Y.; Zheng,
L.; Zheng, X.; Xiao, D.; Wang, S.; Ai,
Keywords: pectin; extraction; passion fruit; steam explosion; ultrasonic; emulsion stability
B.; Sheng, Z. Extraction of Pectin from
Passion Fruit Peel: Composition,
Structural Characterization and
Emulsion Stability. Foods 2022, 11,
1. Introduction
3995. https://doi.org/10.3390/
foods11243995 Passion fruit, in increasing demand yearly, is widely grown in many countries. The
fleshy passion fruit pulp is commonly used to prepare juices and jams [1–3]. During this
Academic Editors: Sara Ghorbani
production, many by-products are produced, especially the peel, which accounts for about
Gorji and Paul J. A. Sobral
50–60% of the total fruit mass. How to use and improve the value of passion fruit peel has
Received: 29 October 2022 attracted much attention [4].
Accepted: 5 December 2022 Passion fruit peel is rich in pectin. Pectin is a complex polysaccharide, mainly com-
Published: 9 December 2022 posed of a galacturonic acid (GalA) main chain and a neutral sugar side chain. Its main
Publisher’s Note: MDPI stays neutral
domains are homogalacturonans (HG), rhamnogalacturonan I (RG–I) and rhamnogalac-
with regard to jurisdictional claims in
turonan II (RG–II) [5]. GalA residue in the HG backbone can be methylated at C–6 or
published maps and institutional affil- acetylated at O–2 and/or O–3 [6]. Pectin is often used as a gelling agent, thickener and
iations. stabilizer in food, pharmaceuticals and cosmetics [7]. Passion fruit peel is a good source
for extracting pectin. Scholars have obtained pectin with an extraction yield of 6.20–18.2%
from passion fruit peel through different extraction methods [8–12].
Acid extraction (AE) is a traditional commercial pectin extraction method. Its process
Copyright: © 2022 by the authors. is mature, but the extraction time is longer than 60 min, and its performance cannot fully
Licensee MDPI, Basel, Switzerland. meet the needs of modern industry. Therefore, scholars have developed many novel
This article is an open access article pectin extraction technologies, such as ultrasound, microwave, ohmic heating, pulsed
distributed under the terms and electric field, high pressure, high-speed shearing and other emerging technologies and
conditions of the Creative Commons
their combinations [12,13]. Ultrasonic-assisted acid extraction (UA), a method to improve
Attribution (CC BY) license (https://
resource efficiency, has been applied to the extraction of pectin by scholars. De Oliveira
creativecommons.org/licenses/by/
et al. [10] obtained pectin with an extraction yield of 12.7% from passion fruit peel using
4.0/).

Foods 2022, 11, 3995. https://doi.org/10.3390/foods11243995 https://www.mdpi.com/journal/foods


Foods 2022, 11, 3995 2 of 12

the UA method. Tran et al. [14] obtained pectin with a yield of 53.8% from papaya at a UA
time of 35 min, higher than AE for 100 min. Maran et al. [15] used a UA time of 27 min to
obtain pectin with a yield of 9.0% from Musa balbisiana.
Steam explosion (SE) is an efficient new heat treatment technology [16]. The principle
of SE is that biomass undergoes high-pressure steam and then instantaneously depressur-
izes, opening the biomass structure and releasing small molecular substances [17]. Studies
have shown that SE has a high extraction yield in the extraction of bioactive components,
such as phenols [18], flavonoids [19] and monosaccharides [20].
Pectin is gradually being accepted as a food emulsifier. The emulsifying and emulsion
stability properties of pectin have attracted much attention in recent years. The emulsifying
properties of pectin are closely related to the extraction method and the source of pectin [21].
Schmidt et al. [22] studied citrus pectin’s interfacial and emulsifying properties with different
esterification degrees. Chen et al. [23] obtained pectin with excellent emulsification at a low
concentration by the AE method from fruit dragon peel. Liu et al. [24] compared the structure
and emulsifying properties of Gaertn seed pectin, apple pectin and citrus pectin. In summary,
the emulsifying properties of pectin are related to the domain, protein content, degree of
esterification, molecular weight and other pectin structures of pectin molecules [25].
This study compared the pectin extraction yield of AE, UA, steam explosion pretreat-
ment combined with acid extraction (SEA) and ultrasonic-assisted SEA (USEA). Then, the
following research was conducted: (1) characterization of the protein content, total phe-
nol content (TPC), degree of esterification (DE), morphological characteristics, molecular
weight (Mw ), Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD)
of pectin; (2) determination of pectin’s thermal and emulsifying properties and clarification
of the relationship between properties and structure. This work aims to obtain a pectin
extraction method from passion fruit peel with high yield and good emulsifying stability.

2. Materials and Methods


2.1. Materials
Purple passion fruit peel was collected in Haikou, China. The passion fruit peel was
cut into small pieces, treated in a water bath at 90 ◦ C for 3 min and dried at 45 ◦ C for
48 h. The dried peel was crushed and collected with a 40-mesh sieve to obtain the dried
peel powder. GalA, arabinose (Ara), galactose (Gal), rhamnose (Rha), xylose (Xyl), glucose
(Glc), mannose (Man) and other standards were purchased from Sigma-Aldrich (Shanghai)
Trading Co., Ltd., Shanghai, China. Other chemicals and solvents are of analytical grade.

2.2. Pectin Extraction


2.2.1. Acid Extraction (AE)
The AE process of pectin followed the method of Kulkarni et al. [26] with slight
modifications. The dried peel powder was treated with a ratio of 1:30 HNO3 (pH 2.0)
at 98 ◦ C for 60 min. After vacuum filtration, the filtrate was concentrated by rotary
evaporation to a quarter of the original volume. Then, a 3-fold volume of ethanol (95% v/v)
was added and stood for 24 h to precipitate pectin. After centrifugation at 4000× g for
10 min, the residue was redissolved with an appropriate amount of distilled water and
loaded in a dialysis bag (20,000 Da). The bag was placed into a large beaker containing a
large amount of distilled water dialyzed for 48 h, concentration by rotary evaporation and
freeze drying were performed to obtain purified pectin.

2.2.2. Ultrasonic-Assisted Acid Extraction (UA)


UA of pectin was performed according to the method of de Oliveira et al. [10] and
slightly modified. The dried peel powder was treated with a ratio of 1:30 HNO3 (pH 2.0)
by an ultrasonic cleaner (JP-080B, Jiemeng Cleaning Equipment Co., Ltd., Shenzhen, China)
under 480 W and 65 ◦ C continuous ultrasound for 15 min. Pectin precipitation, purification
and drying steps were the same as in Section 2.2.1.
Foods 2022, 11, 3995 3 of 12

2.2.3. Steam Explosion Pretreatment Combined with Acid Extraction (SEA)


Pretreatment of dried peel refers to the method of Zhang et al. [27] with minor modifi-
cations. Dried peel (70 g) broken up in advance was loaded into the reaction chamber of an
SE unit (QBS-80; Zheng Dao Co., Ltd., Hebei, China) and then the reaction door was closed
to create a closed space. The peel was placed under steam at 0.6 MPa for 120 s, then the
explosion was completed at 0.0875 s. After SE treatment, the sample was dried at 45 ◦ C for
48 h and through a 40-mesh sieve after high-speed crushing. The pectin extraction steps
were the same as in Section 2.2.1.

2.2.4. Ultrasonic-Assisted Steam Explosion Pretreatment Combined with Acid


Extraction (USEA)
SE pretreatment of peel reference Section 2.2.3 and pectin extraction steps were the
same as in Section 2.2.2.

2.3. Yield
The yield of pectin was calculated with reference to Muñoz-Almagro et al. [28]. The
yield of pectin was calculated using the following formula:

weight of dried pectin


Yield (%) = × 100 (1)
weight of dried powder

2.4. Protein Content and TPC


Determination of protein content in pectin was based on protein binding to Coomassie
brilliant blue G-250 with maximum light absorption at 595 nm [29]. TPC determination
was the gallic acid equivalent obtained using the Folin–Ciocalteu colorimetric method [30].

2.5. Structure Analysis of Pectin


2.5.1. Scanning Electron Microscopy (SEM)
The morphology of the pectin was observed by an SEM (S-3000N, Hitachi Co., Ltd.,
Tokyo, Japan). Pectin was fixed on the sample stage and sprayed with a thin layer of gold.
Next, the pectin samples were placed under an SEM at an accelerating voltage of 10.0 kV.

2.5.2. Determination of Degree of Esterification (DE) Value


The DE of pectin was determined following the method of Kazemi et al. [31]. Pectin
(0.2 g) was wet with 2 mL of anhydrous ethanol and diluted with distilled water to 20 mL.
Five drops of phenolphthalein indicator solution were added and titrated with 0.1 M NaOH
until pink appeared and did not fade within 30 s as the titration endpoint. The volume of
consumed NaOH solution was recorded and denoted as V1 . Then, 10 mL of 0.1 M NaOH
solution was added to a thermostatic oscillator, shaken at 180 rpm for 2 h at 30 ◦ C and
10 mL of 0.1 M HCl solution was added as the end. After adding 5 drops of phenolphthalein
indicator solution, the pectin was titrated with 0.1 M NaOH solution until pink appears
and does not fade within 30 s. The consumption of NaOH was recorded, denoted as V2 .
The DE of pectin was calculated using the following equation:

V2
DE (%) = × 100 (2)
V1 + V2

2.5.3. Monosaccharides Composition


The monosaccharide composition of pectin was tested and slightly modified according
to the method of Hosseini et al. [32]. Pectin was hydrolyzed with 2 M trifluoroacetic acid
(TFA) solution at 100 ◦ C for 2 h. Methanol was added and blow dried with nitrogen. The
dried sample was redissolved with distilled water. We tested using high performance
liquid chromatography (HPLC) equipment (Agilent 1260, Agilent Technologies Co. Ltd.,
Santa Clara, CA, USA) with an AGILENT EC-C18 column (2.1 mm × 50 mm, 2.7 µm)
Foods 2022, 11, 3995 4 of 12

and RI detector. We used 0.005 M sulfuric acid as the mobile phase (the flow rate and
temperature of the mobile phase were 0.8 mL/min and 70 ◦ C, respectively). GalA, Ara,
Gal, Rha, Glc, Gal, Xyl and Man were used as standard. The proportion of HG and RG–I
regions of pectins were calculated according to Yang et al. [6], using the following formula:

HG = GalA − Rha (3)

RG–I = (GalA − HG) + Rha + Gal + Ara (4)

2.5.4. Molecular Weight (Mw )


The Mw of the pectin was tested using an HPLC apparatus (Waters e2695, Wa-
ters Co., Ltd., Milford, MA, USA) equipped with two super hydrogel linear columns
(7.8 mm × 300 mm) and connected in series with the Waters 2414 RI detector. The flow rate
of the mobile phase (0.05% sodium azide solution) was 0.6 mL/min at 40 ◦ C.

2.5.5. FT-IR Spectroscopy


The sample was dried to constant weight, and about 1 mg of pectin was mixed
with potassium bromide at a ratio of 1:50 and then tableted. The infrared region of
400–4000 cm−1 in the FT-IR spectrometer (Tensor27, BRUKER Co., Ltd., Karlsruhe, Germany)
was scanned 16 times with a scanning resolution of 4 cm−1 .

2.5.6. XRD Measurement


The crystal structures of the samples were determined using XRD-6100 (SHIMADZU,
Kyoto, Japan) at an accelerating voltage and current of 40 kV and 30 mA. The X-ray diffraction
pattern is scanned at a diffraction angle (2θ) of 10–60◦ to obtain data at a scan rate of 4◦ /min.

2.6. Thermal Analysis


The thermodynamic characteristic (TG/DTG analysis) was measured at a range of
5–600 ◦ C using a thermogravimetric analyzer (Q600, TA Instruments Co., Ltd., New Castle,
DE, USA). The rate of temperature rise was 10 ◦ C/min and at a nitrogen flow rate of
50 mL/min. The temperature and weight of sample changes were continuously recorded
in the heating range.

2.7. Emulsifying Properties


The emulsion was prepared according to the method of Jiang et al. [33]. The completely
dissolved pectin solution was set to gradient concentrations (0.5%, 1.0%, 1.5% and 2.0%, w/v).
Ten milliliters of pectin solution was mixed with the same amount of corn germ oil, and then
homogenized in a high-speed shearing homogenizer (A25, OuHor Mechanical Equipment
Co., Ltd., Shanghai, China) at 14,000 rpm for 2 min to obtain the emulsion. A digital camera
and microscopy observed the differences in emulsion stored in the dark at room temperature
(23–27 ◦ C) for 1 h and 10 days. An upright microscope (Axio scope A1, Carl Zeiss Co., Ltd.,
Oberkochen, Germany) was used to photograph emulsion droplets on the upper layer (2 cm
below the liquid level) after 10 days of storage at room temperature at a magnification of 200×.

2.8. Statistical Analysis


Significant differences were obtained by analysis of variance (ANOVA) followed by
Tukey’s test (p < 0.05). All tests were conducted in triplicate, and the results were expressed
as mean ± standard deviation.

3. Results and Discussion


3.1. Effect of Extraction Method on Yield
The extraction yield of pectin is shown in Table 1. The extraction yield of pectin by
different methods decreased in the order USEA (10.72%) > SEA (9.93%) > UA (6.52%) > AE
(5.28%). Notably, the extraction yield is based on the calculation after dialysis purification. The
Foods 2022, 11, 3995 5 of 12

extraction yield of pectin was greatly improved after SE pretreatment of passion fruit peel. The
high-pressure steam treated by SE degraded some biomass components of the peel, reduced
the internal bond or network strength of the peel molecules and completed the instantaneous
thermal expansion impact material during the pressure relief stage, resulting in material
breakage. The extraction yield of AE and UA has no statistical difference, but the extraction
time was much lower for UA (15 min). The cavitation, thermal and mechanical effects of
ultrasound destroyed the cell wall of the peel and improved the mass transfer efficiency [34,35].
Therefore, the USEA technology is an efficient and high extraction yield method.

Table 1. Extraction yield, protein content and polyphenol content of pectin.

Samples Yield (%) Protein Content (%) TPC (mg GAE/g)


AE 5.28 ± 1.57 b 0.46 ± 0.08 d 8.58 ± 0.47 b
UA 6.52 ± 0.48 b 0.51 ± 0.05 c 9.15 ± 0.35 b
SEA 9.93 ± 0.33 a 0.68 ± 0.04 a 17.55 ± 0.55 a
USEA 10.72 ± 0.39 a 0.62 ± 0.01 b 18.85 ± 0.22 a
TPC, total polyphenol content; AE, acid extraction; UA, ultrasonic-assisted acid extraction; SEA, steam explosion
pretreatment combined with acid extraction; USEA, ultrasonic-assisted steam explosion pretreatment combined
with acid extraction. The meanings of AE, UA, SEA and USEA in subsequent charts and tables are described
above. Values with different superscripts within a column are significantly different (p < 0.05).

3.2. Protein Content and TPC


As shown in Table 1, the protein content and TPC of pectin using USEA and SEA
were significantly higher than those of UA and AE. At the same time, the ultrasonic
process had only a small effect on protein content and TPC. Studies have shown that pectin
protein positively impacts its emulsifying properties and TPC content closely affects the
antioxidant properties of pectin [6,32]. Therefore, USEA technology may be one way to
improve pectin properties.

3.3. Structural Characteristics of Pectin


3.3.1. Morphology
The morphology of pectin is shown in Figure 1. The surfaces of pectin extracted by
AE and UA are smooth, but there are some typical ultrasonic deep holes in the UA. The
surface of by SEA was uneven and a certain degree of collapse occurred, accompanied
by a certain degree of fragmentation. The pectin extracted by USEA underwent severe
morphological changes, pits appeared to develop on the surface, as well as intense wrinkles,
while producing many small fragments.

Figure 1. Morphology of pectin (×500).


Foods 2022, 11, 3995 6 of 12

3.3.2. DE
The DE value is related to the physicochemical properties of the extracted pectin. As
shown in Table 2, the DE value of pectin recovered from passion fruit peel was 59.31–83.40%,
which belongs to high methoxy pectin [31]. DE of pectin by UA was significantly higher
than that of AE, similar to the results reported by Yang et al. [36], which may be due to
the lower temperature and shorter extraction time of UA in this experiment [10,37]. The
DE values of pectin extracted using SEA and USEA were significantly lower than those
of AE and UA, respectively, which attributed to the high temperature and high-pressure
environment during SE pretreatment [38]. In this study, SE pretreatment did not make
passion fruit pectin become low methoxy pectin, but it significantly reduced the DE value
of pectin. The technology of USEA may positively affect the de-esterification of pectin.

Table 2. DE value, molecular weight and monosaccharide distribution of pectin.

Samples AE UA SEA USEA


a 68.49 ± 0.17 c
DE (%) 74.50 ± 0.86 b 83.40 ± 0.49 59.31 ± 1.72 d
Mw (×105 Da) 6.54 7.18 0.74 0.72
Mw /Mn 1.80 1.65 1.65 1.67
Relative
monosaccharide content
(%, w/w)
GalA 78.41 82.90 74.66 81.26
Ara 15.74 12.20 14.35 12.04
Gal 3.10 2.76 5.61 3.80
Rha 1.39 0.98 1.43 1.30
Xyl 0 0 0 0
Glc 0.82 0.68 2.01 1.04
Man 0.54 0.48 1.94 0.56
HG 77.02 81.92 73.22 79.96
RG–I 21.62 16.92 22.83 18.44
GalA/Rha 56.43 84.62 52.07 62.61
(Ara + Gal)/Rha 13.56 15.27 13.92 12.20
DE, degree of esterification; Mw , molecular weight; Mn, number-average of molar mass; GalA, galacturonic acid;
Ara, arabinose; Gal, galactose; Rha, rhamnose; Xyl, xylose; Glc, glucose; Man, mannose; HG, homogalacturonans;
RG–I, rhamnogalacturonan I. HG = GalA − Rha; RG–I = GalA − HG + Rha + Gal + Ara. Values with different
superscripts in the same row are significantly different (p < 0.05).

3.3.3. Monosaccharide Composition and Mw


Table 2 shows the monosaccharide composition and Mw of pectin. GalA accounts
for 74.66–82.90% of passion fruit pectin monosaccharides. In passion fruit pectin, HG
accounted for the main advantage, indicating that passion fruit pectin is rich in HG (linear)
structure. The HG content of pectin by different extraction methods decreased in the order
UA > USEA > AE > SEA. In contrast, the results of RG–I, opposite to HG, indicate that SE
pretreatment reduced the linear structure of pectin and increased the hair area. Among
them, the pectin extracted by UA and USEA have more linear structures than AE and SEA,
respectively, because the ultrasonic process may lead to the degradation of pectin side
chains [39]. The GalA/Rha ratio shows the difference in the main chains of pectin and the
(Ara + Gal)/Rha reflects the average size of the neutral sugar side chains of pectin [40].
The (Ara + Gal)/Rha of pectin using USEA was the lowest, indicating that the side chain
degradation of the combined process was the most serious. This difference in side chains
may affect the thermal stability of pectin [30].
The functional properties of pectin are closely related to Mw . The mass dispersion
(Mw /Mn ) of all pectin was low, indicating that the Mw of pectin was concentrated. The Mw
of pectin by SEA and USEA were 0.74 × 105 Da and 0.72 × 105 Da, which were much smaller
than AE (6.54 × 105 Da) and UA (7.18 × 105 Da). It seems that high molecular weight
pectin was degraded to low molecular weight during SE pretreatment. The decrease in Mw
of pectin may be related to the thermal degradation and the mechanical damage of instant
Foods 2022, 11, 3995 7 of 12

decompression during SE pretreatment [18,41]. Combined analysis of monosaccharide


composition Mw showed that the side chain and main chain of pectin extracted by SEA
and USEA were seriously degraded at SE pretreatment.

3.3.4. FT-IR and XRD Analysis


FT-IR spectroscopy is a standard method to study the changes in pectin functional
groups. The passion fruit pectin has a typical pectin FT-IR spectrum, as shown in Figure 2.
The intense absorption peak near 3386 cm−1 and the weak absorption peak at 2921 cm−1
is generated by the stretching vibration of O–H and C–H (including CH, CH2 , CH3 ) of
pectin [42]. The absorption peaks near 1739 cm−1 and 1628 cm−1 were produced by the
absorption esterification of esterified carboxyl (–COOR) and ionized carboxyl (–COO–),
respectively. The “fingerprint region” of polysaccharides was 800–1300 cm−1 , and the
bands between 1107 cm−1 and 1014 cm−1 were related to furanose and α–and β–pyranose
rings in pectin samples [43]. The fingerprint regions of pectin extracted by SEA and USEA
were similar, with more pyranose rings than AE and UA.

Figure 2. FT-IR spectra (a) and XRD patterns (b) of pectin.

Figure 2 shows the XRD pattern of passion fruit pectin. The passion fruit pectin has
a semi-crystalline structure. There are two broad peaks near 13.8◦ and 21.1◦ . In addition,
a small part of the crystal structure is shown at 21.7◦ , 22.9◦ and 12.5◦ . The results are
similar to those reported for pectin from sunflowers [44] and sweet lemon [45]. The crystal
structures of pectin extracted by AE and SEA are similar but different from UA and USEA.
It shows that SE pretreatment has little effect on the crystal structure of pectin, while
the ultrasonic-assisted process changes the crystal structure of pectin. The difference in
peak shape of XRD patterns between ultrasonically and thermally treated pectin was also
reported [46].

3.4. Thermal Analysis of Pectin


The thermal analysis provides information on the thermal stability of polymer ma-
terials [47]. Figure 3 shows the TG and DTG curves of different passion fruit pectin. The
thermal weight loss of pectin was divided into three regions: 50–160 ◦ C, 160–400 ◦ C and
400–600 ◦ C. In the first region, the weight of pectin is slightly reduced and the maximum
mass loss speed was at nearly 90.0 ◦ C, shown in the DTG image. It is caused by the evap-
oration of free water and bound water in pectin [48]. In the second region, the weight of
pectin extracted by AE, UA and USEA decreased by 55.2%, 56.1% and 55.2%, respectively,
while SEA decreased by 50.8%. For DTG, the maximum mass loss temperatures of pectin
obtained from AE and UA were 238 ◦ C, while those of SEA and USEA were 211 ◦ C and
241 ◦ C. It should be noted that although the maximum mass loss speed temperatures of
SEA and USEA were lower than those of AE and UA, their loss began at a lower tempera-
Foods 2022, 11, 3995 8 of 12

ture. The pectin obtained by USEA and SEA was more susceptible to thermal degradation
mainly due to the decrease of Mw of pectin by SE treatment [23]. The change in the second
region can be explained by the thermal degradation of the galacturonic acid chain, the
decarboxylation of the acid side group and the carbon in the ring to generate different
gaseous products and solid char [49]. The third region shows a slow weight loss, which
may be due to the slow thermal decomposition of solid carbon due to the continuous
temperature increase. In general, SE pretreatment reduced the thermal stability of passion
fruit pectin.

Figure 3. Thermodynamic characteristic of pectin.

3.5. Emulsifying Properties of Pectin


The digital photos of the emulsions after storage for 1 h and 10 days at room tempera-
ture are shown in Figure 4a. After 1 h of preparation, some pectin emulsions (AE–0.5%,
UA–1.0%, UA–0.5% and all SEA and USEA pectin emulsions) had different degrees of
phase separation. During the storage process (Figure S1), it can be seen that the creaming
index of pectin emulsions changed significantly in the short term after preparation and
related to the concentration of pectin. It is worth noting that the pectin emulsions (except
for UA) had little change in the creaming index during subsequent storage. The higher
concentration of pectin led to a higher stability of emulsions only in short timeframes due
to the increase in viscosity. However, the concentration did not have an effect at longer
times [33]. For SEA and USEA pectin emulsions, more phase separation occurred in the
early stage of storage, which can be resolved as the lower viscosity of the pectin emulsion
was caused by lower Mw . In addition, the pectin emulsion stability of UA was lower than
that of other methods, which may be related to its lower RG–I content [23].
Figure 4b shows optical microscope images of droplets in the upper layer of the
emulsions after storage for 10 days at room temperature. The pectin emulsions of UA can
only be observed with less or no droplets. However, the pectin emulsions of SEA and
USEA can still see dense and tiny droplets in the concentration of pectin solutions at 1.0%,
1.5% and 2.0%. According to Stoke’s law, the pectin emulsions of SEA and USEA with
smaller droplet sizes may have better emulsion stability [33]. The emulsion stability of SEA
and USEA pectin during long-term storage may be related to their high protein and RG–I
content which mediates the intermolecular association between adsorbed pectin chains to
prevent droplet coalescence [50].
Foods 2022, 11, 3995 9 of 12

Figure 4. Emulsifying properties of pectin. (a) The appearance of emulsions after storage for 1 h and
10 days at room temperature; (b) optical microscope images of droplets in the upper layer of the
emulsions after storage for 10 days at room temperature (×200).
Foods 2022, 11, 3995 10 of 12

4. Conclusions
This study compared four processes for extracting pectin from passion fruit peel.
The UA process improved the extraction efficiency and obtained a higher DE value and
Mw pectin but reduced the proportion of RG–I of pectin, resulting in the pectin emulsion
stability not being as good as that of the AE. SE pretreatment significantly improved the
extraction yield of pectin and obtained a lower DE value and lower Mw of pectin (SEA and
USEA). The pectin extracted by SEA and USEA has higher protein content, TPC and RG–I
structure and has better emulsion stability, but reduces the thermal stability of pectin. In
general, USEA combines the high efficiency of UA and the high extraction yield of SEA,
and the pectin obtained by this method has good pectin emulsion stability. This study
provides a pectin extraction method with a high yield and good emulsifying properties
from passion fruit peel.

Supplementary Materials: The following supporting information can be downloaded at: https:
//www.mdpi.com/article/10.3390/foods11243995/s1, Figure S1: The creaming index of pectin
emulsions for 10 days at room temperature.
Author Contributions: Conceptualization, Z.S.; methodology, Y.L., Y.Y., B.A., Z.S.; investigation, Y.L.,
Y.Y., B.A., Z.S., L.Z., D.X., X.Z. and S.W.; data curation, Y.L., Y.Y., B.A.; visualization, Y.L., Y.Y.; formal
analysis, Y.L., Y.Y., B.A., L.Z., D.X., X.Z. and S.W.; writing—original draft, Y.L., Y.Y., Z.S.; project
administration, B.A.; writing—review and editing, B.A., Z.S.; funding acquisition, Z.S.; resources, Z.S.
All authors have read and agreed to the published version of the manuscript.
Funding: This research was funded by the Natural Science Foundation of Hainan Province,
China (320CXTD440), the Key Research and Development Program of of Hainan Province, China
(ZDYF2020173), and the Central Public-interest Scientific Institution Basal Research Fund for Innova-
tive Research Team Program of CATAS, China (1630092022003).
Data Availability Statement: Data is contained within the article or Supplementary Materials.
Conflicts of Interest: The authors declare no conflict of interest.

References
1. Corrêa, R.C.G.; Peralta, R.M.; Haminiuk, C.W.I.; Maciel, G.M.; Bracht, A.; Ferreira, I.C.F.R. The past decade findings related with
nutritional composition, bioactive molecules and biotechnological applications of Passiflora spp. (passion fruit). Trends Food Sci.
Technol. 2016, 58, 79–95. [CrossRef]
2. My-Thao Nguyen, T.; Anh-Thu Nguyen, T.; Tuong-Van Pham, N.; Ly, Q.-V.; Thuy-Quynh Tran, T.; Thach, T.-D.; Nguyen, C.-L.;
Banh, K.-S.; Le, V.-D.; Nguyen, L.-P.; et al. Biosynthesis of metallic nanoparticles from waste Passiflora edulis peels for their
antibacterial effect and catalytic activity. Arab. J. Chem. 2021, 14, 103096. [CrossRef]
3. Fonseca, A.M.A.; Geraldi, M.V.; Junior, M.R.M.; Silvestre, A.J.D.; Rocha, S.M. Purple passion fruit (Passiflora edulis f. edulis): A
comprehensive review on the nutritional value, phytochemical profile and associated health effects. Food Res. Int. 2022, 160,
111665. [CrossRef]
4. Delvar, A.; de Caro, P.; Candy, L.; Caro, Y.; Sing, A.S.C.; Raynaud, C. Integrated process for extraction and formulation in
emulsions of active molecules from fresh passion fruits (Passiflora edulis Sims). J. Food Eng. 2019, 263, 388–397. [CrossRef]
5. Adetunji, L.R.; Adekunle, A.; Orsat, V.; Raghavan, V. Advances in the pectin production process using novel extraction techniques:
A review. Food Hydrocoll. 2017, 62, 239–250. [CrossRef]
6. Yang, J.S.; Mu, T.H.; Ma, M.M. Extraction, structure, and emulsifying properties of pectin from potato pulp. Food Chem. 2018, 244,
197–205. [CrossRef]
7. Klinchongkon, K.; Khuwijitjaru, P.; Adachi, S. Properties of subcritical water-hydrolyzed passion fruit (Passiflora edulis) pectin.
Food Hydrocoll. 2018, 74, 72–77. [CrossRef]
8. De Oliveira, C.F.; Giordani, D.; Gurak, P.D.; Cladera-Olivera, F.; Marczak, L.D.F. Extraction of pectin from passion fruit peel using
moderate electric field and conventional heating extraction methods. Innov. Food Sci. Emerg. Technol. 2015, 29, 201–208. [CrossRef]
9. De Oliveira, C.F.; Gurak, P.D.; Cladera-Olivera, F.; Marczak, L.D.F.; Karwe, M. Combined Effect of High-Pressure and Conventional
Heating on Pectin Extraction from Passion Fruit Peel. Food Bioprocess Technol. 2016, 9, 1021–1030. [CrossRef]
10. De Oliveira, C.F.; Giordani, D.; Lutckemier, R.; Gurak, P.D.; Cladera-Olivera, F.; Ferreira Marczak, L.D. Extraction of pectin from
passion fruit peel assisted by ultrasound. LWT Food Sci. Technol. 2016, 71, 110–115. [CrossRef]
11. Seixas, F.L.; Fukuda, D.L.; Turbiani, F.R.B.; Garcia, P.S.; Petkowicz, C.L.D.O.; Jagadevan, S.; Gimenes, M.L. Extraction of pectin
from passion fruit peel (Passiflora edulis f. flavicarpa) by microwave-induced heating. Food Hydrocoll. 2014, 38, 186–192. [CrossRef]
Foods 2022, 11, 3995 11 of 12

12. Lin, Y.P.; An, F.P.; He, H.; Geng, F.; Song, H.B.; Huang, Q. Structural and rheological characterization of pectin from passion fruit
(Passiflora edulis f. flavicarpa) peel extracted by high-speed shearing. Food Hydrocoll. 2021, 114, 106555. [CrossRef]
13. Gavahian, M.; Mathad, G.N.; Pandiselvam, R.; Lin, J.; Sun, D.-W. Emerging technologies to obtain pectin from food processing
by-products: A strategy for enhancing resource efficiency. Trends Food Sci. Technol. 2021, 115, 42–54. [CrossRef]
14. Tran, T.T.B.; Saifullah, M.; Nguyen, N.H.; Nguyen, M.H.; Vuong, Q.V. Comparison of ultrasound-assisted and conventional
extraction for recovery of pectin from Gac (Momordica cochinchinensis) pulp. Future Foods 2021, 4, 100074. [CrossRef]
15. Maran, J.P.; Priya, B.; Al-Dhabi, N.A.; Ponmurugan, K.; Moorthy, I.G.; Sivarajasekar, N. Ultrasound assisted citric acid mediated
pectin extraction from industrial waste of Musa balbisiana. Ultrason. Sonochem. 2017, 35, 204–209. [CrossRef]
16. Chen, Y.; Shan, S.; Cao, D.; Tang, D. Steam flash explosion pretreatment enhances soybean seed coat phenolic profiles and
antioxidant activity. Food Chem. 2020, 319, 126552. [CrossRef] [PubMed]
17. Martin-Sampedro, R.; Capanema, E.A.; Hoeger, I.; Villar, J.C.; Rojas, O.J. Lignin changes after steam explosion and laccase-
mediator treatment of eucalyptus wood chips. J. Agric. Food Chem. 2011, 59, 8761–8769. [CrossRef]
18. Wan, F.C.; Feng, C.F.; Luo, K.Y.; Cui, W.Y.; Xia, Z.H.; Cheng, A.W. Effect of steam explosion on phenolics and antioxidant activity
in plants: A review. Trends Food Sci. Technol. 2022, 124, 13–24. [CrossRef]
19. Hong, Q.Y.; Chen, G.J.; Wang, Z.R.; Chen, X.H.; Shi, Y.; Chen, Q.L.; Kan, J.Q. Impact of processing parameters on physicochemical
properties and biological activities of Qingke (highland hull-less barley) treated by steam explosion. J. Food Process. Preserv. 2020,
44, e14793. [CrossRef]
20. Rojas-Pérez, L.C.; Narváez-Rincón, P.C.; Ballesteros, I. Improving sugar extraction from brewers’ spent grain using sequential
deproteinization and acid-catalyzed steam explosion in a biorefinery context. Biomass Bioenergy 2022, 159, 106389. [CrossRef]
21. Cui, J.; Zhao, C.; Feng, L.; Han, Y.; Du, H.; Xiao, H.; Zheng, J. Pectins from fruits: Relationships between extraction methods,
structural characteristics, and functional properties. Trends Food Sci. Technol. 2021, 110, 39–54. [CrossRef]
22. Schmidt, U.S.; Schütz, L.; Schuchmann, H.P. Interfacial and emulsifying properties of citrus pectin: Interaction of pH, ionic
strength and degree of esterification. Food Hydrocoll. 2017, 62, 288–298. [CrossRef]
23. Chen, H.; Liu, Y.; Zhang, J.; Jiang, Y.; Li, D. Pectin extracted from dragon fruit Peel: An exploration as a natural emulsifier. Int. J.
Biol. Macromol. 2022, 221, 976–985. [CrossRef] [PubMed]
24. Liu, H.; Deng, L.; Dai, T.; Chen, J.; Liu, W.; Liu, C.; Chen, M.; Liang, R. Emulsifying and emulsion stabilization mechanism of
pectin from Nicandra physaloides (Linn.) Gaertn seeds: Comparison with apple and citrus pectin. Food Hydrocoll. 2022, 130, 107674.
[CrossRef]
25. Ngouémazong, E.D.; Christiaens, S.; Shpigelman, A.; Van Loey, A.; Hendrickx, M. The Emulsifying and Emulsion-Stabilizing
Properties of Pectin: A Review. Compr. Rev. Food Sci. Food Saf. 2015, 14, 705–718. [CrossRef]
26. Kulkarni, S.G.; Vijayanand, P. Effect of extraction conditions on the quality characteristics of pectin from passion fruit peel
(Passiflora edulis f. flavicarpa L.). LWT Food Sci. Technol. 2010, 43, 1026–1031. [CrossRef]
27. Zhang, S.Y.; Zheng, L.L.; Zheng, X.Y.; Ai, B.L.; Yang, Y.; Pan, Y.G.; Sheng, Z.W. Effect of steam explosion treatments on the
functional properties and structure of camellia (Camellia oleifera Abel.) seed cake protein. Food Hydrocoll. 2019, 93, 189–197.
[CrossRef]
28. Munoz-Almagro, N.; Valadez-Carmona, L.; Mendiola, J.A.; Ibanez, E.; Villamiel, M. Structural characterisation of pectin obtained
from cacao pod husk. Comparison of conventional and subcritical water extraction. Carbohydr. Polym. 2019, 217, 69–78. [CrossRef]
[PubMed]
29. Lin, Z.; Fischer, J.; Wicker, L. Intermolecular binding of blueberry pectin-rich fractions and anthocyanin. Food Chem. 2016, 194,
986–993. [CrossRef] [PubMed]
30. Hu, W.; Chen, S.; Wu, D.; Zhu, K.; Ye, X. Physicochemical and macromolecule properties of RG-I enriched pectin from citrus
wastes by manosonication extraction. Int. J. Biol. Macromol. 2021, 176, 332–341. [CrossRef] [PubMed]
31. Kazemi, M.; Khodaiyan, F.; Hosseini, S.S. Eggplant peel as a high potential source of high methylated pectin: Ultrasonic extraction
optimization and characterization. LWT Food Sci. Technol. 2019, 105, 182–189. [CrossRef]
32. Hosseini, S.S.; Khodaiyan, F.; Kazemi, M.; Najari, Z. Optimization and characterization of pectin extracted from sour orange peel
by ultrasound assisted method. Int. J. Biol. Macromol. 2019, 125, 621–629. [CrossRef]
33. Jiang, Y.; Xu, Y.H.; Li, F.; Li, D.P.; Huang, Q.R. Pectin extracted from persimmon peel: A physicochemical characterization and
emulsifying properties evaluation. Food Hydrocoll. 2020, 101, 105561. [CrossRef]
34. Tiwari, B.K. Ultrasound: A clean, green extraction technology. TrAC Trends Anal. Chem. 2015, 71, 100–109. [CrossRef]
35. Miano, A.C.; Ibarz, A.; Augusto, P.E. Mechanisms for improving mass transfer in food with ultrasound technology: Describing
the phenomena in two model cases. Ultrason. Sonochem. 2016, 29, 413–419. [CrossRef] [PubMed]
36. Yang, Y.S.; Wang, Z.M.; Hu, D.; Xiao, K.J.; Wu, J.Y. Efficient extraction of pectin from sisal waste by combined enzymatic and
ultrasonic process. Food Hydrocoll. 2018, 79, 189–196. [CrossRef]
37. Basak, S.; Annapure, U.S. Trends in “green” and novel methods of pectin modification—A review. Carbohydr. Polym. 2022, 278,
118967. [CrossRef]
38. Guo, X.B.; Guo, X.M.; Meng, H.C.; Zhang, B.B.; Yu, S.J. Using the high temperature resistant pH electrode to auxiliarily study the
sugar beet pectin extraction under different extraction conditions. Food Hydrocoll. 2017, 70, 105–113. [CrossRef]
Foods 2022, 11, 3995 12 of 12

39. Chen, S.; Xiao, L.; Li, S.; Meng, T.; Wang, L.; Zhang, W. The effect of sonication-synergistic natural deep eutectic solvents on
extraction yield, structural and physicochemical properties of pectins extracted from mango peels. Ultrason. Sonochem. 2022, 86,
106045. [CrossRef]
40. Zhang, L.; Ye, X.; Xue, S.J.; Zhang, X.; Liu, D.; Meng, R.; Chen, S. Effect of high-intensity ultrasound on the physicochemical
properties and nanostructure of citrus pectin. J. Sci. Food Agric. 2013, 93, 2028–2036. [CrossRef]
41. Liu, C.Y.; Sun, Y.Y.; Jia, Y.Q.; Geng, X.Q.; Pan, L.C.; Jiang, W.; Xie, B.Y.; Zhu, Z.Y. Effect of steam explosion pretreatment on
the structure and bioactivity of Ampelopsis grossedentata polysaccharides. Int. J. Biol. Macromol. 2021, 185, 194–205. [CrossRef]
[PubMed]
42. Chen, Y.; Zhang, J.G.; Sun, H.J.; Wei, Z.J. Pectin from Abelmoschus esculentus: Optimization of extraction and rheological properties.
Int. J. Biol. Macromol. 2014, 70, 498–505. [CrossRef] [PubMed]
43. Xu, F.; Zhang, S.; Waterhouse, G.I.N.; Zhou, T.; Du, Y.; Sun-Waterhouse, D.; Wu, P. Yeast fermentation of apple and grape pomaces
affects subsequent aqueous pectin extraction: Composition, structure, functional and antioxidant properties of pectins. Food
Hydrocoll. 2022, 133, 107945. [CrossRef]
44. Ezzati, S.; Ayaseh, A.; Ghanbarzadeh, B.; Heshmati, M.K. Pectin from sunflower by-product: Optimization of ultrasound-assisted
extraction, characterization, and functional analysis. Int. J. Biol. Macromol. 2020, 165, 776–786. [CrossRef] [PubMed]
45. Rahmani, Z.; Khodaiyan, F.; Kazemi, M.; Sharifan, A. Optimization of microwave-assisted extraction and structural characteriza-
tion of pectin from sweet lemon peel. Int. J. Biol. Macromol. 2020, 147, 1107–1115. [CrossRef] [PubMed]
46. Qin, C.; Yang, G.; Zhu, C.; Wei, M. Characterization of edible film fabricated with HG-type hawthorn pectin gained using different
extraction methods. Carbohydr. Polym. 2022, 285, 119270. [CrossRef] [PubMed]
47. Muthukumaran, C.; Kanmani, B.; Sharmila, G.; Kumar, M.; Shanmugaprakash, M. Carboxymethylation of pectin: Optimization,
characterization and in-vitro drug release studies. Carbohydr. Polym. 2018, 194, 311–318. [CrossRef]
48. Sucheta; Misra, N.N.; Yadav, S.K. Extraction of pectin from black carrot pomace using intermittent microwave, ultrasound and
conventional heating: Kinetics, characterization and process economics. Food Hydrocoll. 2020, 102, 105592. [CrossRef]
49. Wang, W.J.; Ma, X.B.; Jiang, P.; Hu, L.L.; Zhi, Z.J.; Chen, J.L.; Ding, T.; Ye, X.Q.; Liu, D.H. Characterization of pectin from grapefruit
peel: A comparison of ultrasound-assisted and conventional heating extractions. Food Hydrocoll. 2016, 61, 730–739. [CrossRef]
50. Funami, T.; Nakauma, M.; Ishihara, S.; Tanaka, R.; Inoue, T.; Phillips, G.O. Structural modifications of sugar beet pectin and the
relationship of structure to functionality. Food Hydrocoll. 2011, 25, 221–229. [CrossRef]

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