Food Chemistry 286 (2019) 1–7

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

Research Article

Efficient extraction and characterization of pectin from orange peel by a T

combined surfactant and microwave assisted process
⁎
Dong-Lin Sua,b,e, Pei-Jun Lib,d, , Siew Young Quekc,e, Zhi-Qin Huangd, Yu-Jun Yuand,
⁎
Gao-Yang Lib,e, Yang Shana,b,e,
a
Longping Branch Graduate School, Central South University, Changsha 410125, China
b
Hunan Agricultural Product Processing Institute, Hunan Academy of Agricultural Sciences, Changsha 410125, China
c
Food Science, School of Chemical Sciences, The University of Auckland, Private Bag 92019, Auckland 1142, New Zealand
d
Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guilin
541004, China
e
International Joint Laboratory on Fruits & Vegetables Processing and Quality Safety, Changsha 410125, China

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

Chemical compounds studied in this article: Surfactant and microwave assisted extraction (S-MAE) was used for pectin extraction from orange peel. First, we
D-(+)-glucose (PubChem CID: 5793) optimized the conditions of microwave assisted extraction (MAE), e.g., irradiation time, liquid-to-solid ratio
D-(+)-galacturonic acid (PubChem CID: (LSR), and pH on pectin yield (PY), galacturonic acid (GA) content, and degree of esterification (DE) using a Box-
152867) Behnken design. Under optimal conditions (pH 1.2, 7.0 min, and 21.5 v/w LSR), we obtained a PY of
Sodium hydroxide (PubChem CID: 14798)
28.0 ± 0.5%, which was close to the predicted value (31.1%). Second, we analyzed the effect of surfactant on
Ethanol (PubChem CID: 702)
microwave extraction of pectin. Among the surfactants investigated, Tween-80 (8 g/L, w/v) increased PY by
Hydrochloric acid (PubChem CID: 313)
Tween-80 (PubChem CID: 5281955) 17.0%. Compared with conventional solvent extraction, S-MAE is a novel and efficient method for pectin ex-
Tween-20 (PubChem CID: 443314) traction, which generated a higher (p < 0.05) PY (32.8%), GA content (78.1%), DE (69.8%), and Mw
Sodium dodecyl sulfate (PubChem CID: (286.3 kDa).
3423265)
Polyethylene glycol (PubChem CID: 174)
Carbazole (PubChem CID: 6854)
Keywords:
Surfactant
Microwave assisted extraction
Orange peel pectin
Optimization
Extraction

1. Introduction
Pectin is a polysaccharide present in the cell wall and middle la-
mellae of several land-growing plants, especially fruit and vegetable
crops. D-Galacturonic acid is the main monomeric unit of pectin
(Adetunji, Adekunle, Orsat, & Raghavan, 2017). Commercial natural
pectin is derived from apple pomace and citrus peel, which are both by-
products of juice (Jamsazzadeh Kermani, Shpigelman, Pham, Van Loey,
& Hendrickx, 2015). Pectin is mainly used as a gelling, stabilizing, and
thickening agent in food systems. Additionally, pectin may reduce the
incidence of heart disease and gallstones (Bagherian, Ashtiani,
Fouladitajar, & Mohtashamy, 2011). It has been reported that pectin
may affect the pasting, rheological, and digestibility properties of corn
starch (Ma et al., 2019).
Pectin is commonly extracted using hot water (60–100 °C) at pH
1.5–3.0 for several hours. However, the conventional extraction (CE)
method is tedious, time consuming, and labor intensive, and may in-
volve either volatile and hazardous organic solvents or strong acid-base
solutions (Huang, Jeffrey, Zhang, & Huang, 2012). Recently, novel
extraction techniques have been used in pectin extraction including
microwave-assisted extraction (MAE) (Swamy & Muthukumarappan,
2017), ultrasound-assisted extraction (Moorthy et al., 2017), subcritical
water extraction (Ueno, Tanaka, Hosino, Sasaki, & Goto, 2008), and
enzyme-assisted extraction (Adetunji et al., 2017). Among them, MAE is

⁎
Corresponding authors at: Hunan Agricultural Product Processing Institute, Hunan Academy of Agricultural Sciences, Changsha 410125, China.
E-mail addresses: lipeijun@glut.edu.cn (P.-J. Li), sy6302@sohu.com (Y. Shan).

https://doi.org/10.1016/j.foodchem.2019.01.200
Received 10 May 2018; Received in revised form 22 January 2019; Accepted 31 January 2019
Available online 08 February 2019
0308-8146/ © 2019 Elsevier Ltd. All rights reserved.
D.-L. Su, et al.
an interesting alternative to conventional extraction methods that offers
significant advantages. Specifically, MAE requires shorter processing
times and less solvent, has higher extraction rates, and is low in cost
(Huang et al., 2012). Therefore, microwave irradiation has been used
for pectin extraction from pectin-rich biomass such as banana peels
(Swamy & Muthukumarappan, 2017), mango peels (Matharu,
Houghton, Lucas-Torres, & Moreno, 2016), pumpkin (Kostalova,
Aguedo, & Hromadkova, 2016), and orange peels (Hosseini, Khodaiyan,
& Yarmand, 2016a, 2016b).
Surfactant-mediated extraction is a novel method for extracting
bioactive compounds including polyphenols (Li, Raza, Wang, Xu, &
Chen, 2017) and lectin (He, Shi, Walid, Ma, & Xue, 2013). Surfactants,
which are amphiphilic molecules with a hydrophilic head and a hy-
drophobic tail, are also known as surface active agents. When the
concentration of surfactant is present at or above its critical micelle
concentration, micelles form. These micelles are capable of establishing
chemical and physical interactions with either hydrophilic or lipophilic
substances (Sharma, Kori, & Parmar, 2015). Pectin belongs to a series of
polysaccharides that have different chemical structures with a wide
range of polarity.
In this study, we evaluated the extraction of orange peel pectin
using MAE and investigated the effect of pH, liquid-to-solid ratio (LSR),
and irradiation time on pectin yield (PY), galacturonic acid (GA) con-
tent, and degree of esterification (DE). Additionally, we established a
novel surfactant-assisted microwave extraction (S-MAE) method for
recovery of pectin from orange peels. Finally, we compared yield and
chemical properties of pectin extracted by MAE, S-MAE, and CE
methods.
2. Materials and methods
2.1. Materials
Dried satsuma mandarin (Citrus unshiu) peels were obtained from
Hailian (Huaihua, Hunan, China). The collected peels were immersed in
water at 90 °C for 5 min to inactivate enzymes and subsequently dried
in an oven with air circulation at 50 °C for 24 h. The dried peels were
milled and passed through a 40-mesh sieve. The pretreated orange peel
powder (OPP) was packed in dark bags and stored in a dry environment
prior to experimental analyses.
All chemical reagents including surfactants, ethanol, and HCl were
of analytical grade and purchased from Sinopharm Chemical Reagent
Co., Ltd. (Shanghai, China). Commodity pectin (CP; S11083, extracted
from orange) and polygalacturonic acid were acquired from Shanghai
Yuanye Bio-Technology Co., Ltd. (Shanghai, China). Monosaccharide
standards were supplied by Aladdin Reagents (Shanghai, China).
2.2. Extraction of pectin from OPP by conventional extraction (CE)
CE conditions were optimized using a single factor experiment (data
not shown). The pH of the extracting agent was adjusted to 1.0 with
0.1 M HCl, LSR was set at 30 (v/w), and the mixture was heated in a
90 °C water bath for 180 min. After extraction, the resulting sediment
was filtered using eight layers of gauze (20 mesh). To separate the re-
maining insoluble material, the solution was centrifuged at 4000 rpm
for 15 min. Pectin was precipitated with the addition of 98% ethanol
(1.5:1, v/v) and left for 6 h. The coagulated pectin was separated by
centrifugation at 4000 rpm for 15 min and washed three times with
60% (v/v) ethanol. The pectin was dried at 50 °C in a laboratory drier
for 12 h (Bagherian et al., 2011). PY was calculated using the following
equation (Santos, Espeleta, Branco, & de Assis, 2013):
Mass of extracted pectin (g)
PY (%) = × 100
Mass of OPP (g) (1)
2
Food Chemistry 286 (2019) 1–7
2.3. Extraction of pectin from OPP using MAE
2.3.1. Determination of microwave powder
Microwave-assisted extraction (MAE) of OPP was performed ac-
cording to the method reported by Seixas, Fukuda, Turbiani, Garcia,
and Petkowicz (2014) with minor modifications. OPP (3 g) was added
to a 500-mL beaker containing an acidic solution. The beaker was
partially covered with a glass lid and subjected to microwave irradia-
tion (2450 MHz, Galanz, G80F20CN2L-B8 [R0], China) for pre-
determined time intervals. To maintain a constant suspension con-
centration, the amount of evaporated water was replenished at regular
intervals. The initial microwave extraction conditions were obtained
using a single factor experiment: pH 1.0 (0.1 M HCl), LSR 25, 6 min
irradiation, and 160–480 W. Subsequently, the conventional extraction
method was performed (see Section 2.2).
2.3.2. Experimental design for RSM and data analysis
Response surface methodology (RSM) and Box-Behnken design
(BBD) were used to determine the optimal conditions for pectin ex-
traction from orange peels. A three-level-three-factor BBD was applied
to explore the best combination of three independent factors affecting
extraction process, including pH (X1: 0.5–1.5), irradiation time (X2:
5–7 min), and LSR (X3: 20–30). The whole design consisted of seventeen
experimental points. The experimental design and data analysis were
performed using Design Expert Software 8.0.6 (Stat Ease Inc.,
Minneapolis, USA). The response variables were fitted to a quadratic
polynomial model (Wang et al., 2015) as shown below,
3 3 2 3
Y = β0 + ∑ βi Xi + ∑ βii Xi2 + ∑ ∑ βij Xi Xj
i=1 i=1 i=1 j=i+1 (2)
where Y is the response variable; β0, βi, βii, and βij are the regression
coefficients for intercept, linearity, square, and interaction, respec-
tively; and Xi and Xj represent the coded independent variables, which
are coded according to the equation
x i = (Xi − −X0 )/ΔXi (3)
where xi is the coded value of the variable Xi; X0 is the value of xi at the
center point; and ΔXi is the change in the real value of the variable i
corresponding to a variation of a unit for the dimensionless value of the
variable i (Prakash Maran & Manikandan, 2012). The actual and coded
levels of the independent variables used in the experimental design are
shown in Table A1 (supplementary material).
2.4. Extraction of pectin from OPP using S-MAE
We studied the synergistic action of surfactants and MAE for pectin
extraction. We evaluated Tween-80, Tween-20, polyethylene glycol
(PEG) 4000, PEG 8000, sucrose fatty acid esters (SE), and sodium do-
decyl sulfate (SDS). Each of tested surfactants (2.0, 4.0, 6.0, 8.0, and
10.0 g/L, w/v) was added to the fresh medium prior to MAE. The MAE
conditions were optimized as reported in Section 3.2: pH 1.2, LSR 21.5,
7.0 min irradiation time, and 400 W. All of the following procedures
were carried out according to Section 2.2.
2.5. Analyses of the extracted pectin
2.5.1. GA content
GA content was determined spectrophotometrically using carbazole
as reported by Kumar and Kumar (2017) with minor modifications.
Briefly, 6 mL of concentrated sulfuric acid (98%) was kept in an ice
bath, and 1.0 mL pectin solution (100 μg/mL) was added. The resulting
mixture was vortexed, heated at 100 °C for 20 min, and cooled to room
temperature. Alcohol-based carbazon (0.6 mL of 0.15%, w/v) was
added. The mixture was vortexed and placed in the dark for 2 h. The
absorbance of the resultant solution was measured at 530 nm. A
D.-L. Su, et al. Food Chemistry 286 (2019) 1–7

Table 1
Box-Behnken experimental designs with experimental data and predicted values. Variables and their levels are shown in Table A1.
Run Independent variables Measured responses Predicted responses

X1a X2b X3 c
PY d
GA e
DE f
PY GA DE

1 1.0 6.0 25.0 27.8 51.0 69.2 27.4 50.8 70.9

2 1.0 5.0 20.0 24.1 50.5 47.4 23.8 50.6 48.8
3 0.5 6.0 30.0 23.9 23.4 44.0 24.1 24.6 43.0
4 1.0 7.0 30.0 27.5 52.6 54.8 27.8 52.6 53.4
5 1.0 6.0 25.0 26.8 49.3 70.4 27.4 50.8 70.9
6 1.0 6.0 25.0 28.3 48.5 70.8 27.4 50.8 70.9
7 1.0 5.0 30.0 23.5 50.3 51.7 23.1 50.8 53.7
8 0.5 6.0 20.0 24.0 27.7 52.4 24.1 29.4 52.0
9 1.5 5.0 25.0 24.0 57.3 72.8 24.5 58.5 70.4
10 1.0 6.0 25.0 26.4 56.0 71.4 27.4 50.8 70.9
11 1.5 6.0 30.0 23.9 61.7 68.0 23.8 60.0 68.5
12 1.0 7.0 20.0 30.3 56.8 68.4 30.7 56.3 66.4
13 1.5 6.0 20.0 27.5 60.1 66.6 27.3 58.9 67.6
14 0.5 5.0 25.0 22.3 30.7 31.7 22.5 29.0 30.7
15 1.0 6.0 25.0 27.5 49.1 72.5 27.4 50.8 70.9
16 0.5 7.0 25.0 29.4 31.0 56.0 28.9 29.8 58.4
17 1.5 7.0 25.0 29.9 63.5 59.0 29.7 65.2 60.0

a
X1: pH.
b
X2: irradiation time.
c
X3: liquid solid ratio.
d
PY: pectin yield.
e
GA: galacturonic acid.
f
DE: degree of esterification.

standard curve was generated using different concentrations
(20–100 μg/mL) of a D-GA standard.
2.5.2. Determination of DE
The DE of pectin samples was determined by titration, as reported
by Jafari, Khodaiyan, Kiani, and Hosseini (2017) with minor mod-
ifications. OPP (30 mg) was dissolved in 30 mL carbon dioxide-free
water at 40 °C. Five drops of phenolphthalein reagent were added, and
the sample was titrated with 0.1 M sodium hydroxide (V1, mL). Sodium
hydroxide (6 mL, 0.5 M) was added, and the sample was allowed to
stand for 15 min. In the next step, 6 mL of 0.5 M hydrochloric acid was
added, and the sample was shaken vigorously until the pink color dis-
appeared. Five drops of phenolphthalein were added again, and the
solution was titrated with 0.1 M sodium hydroxide until a pale pink
color was obtained (V2, mL). DE was calculated using the following
equation,
V2
DE (%) = × 100
V1 + V2
Spectra were recorded using a Nicolet iS10 spectrometer (Thermo
Fisher Scientific, USA) and KBr disk procedure in the 4000–450 cm−1
range.
2.6. Morphology
To visualize the morphology of the OPP samples, scanning electron
microscopy (SEM; Hitachi S-4800) images were taken before and after
the extraction process. The samples were adhered to a support with the
use of a double-sided conductive carbon tape and covered in gold to
ensure electrical conductivity.
2.7. Statistical analysis
Results are expressed as mean ± SD. All experimental data were
analyzed using one-way analysis of variance (ANOVA) and Tukey's test.
Statistical significance was set at p < 0.05.
(4)
3. Results and discussion

2.5.3. Total sugar assay and protein content
Total carbohydrate content was determined as glucose equivalents
according to a modified phenol-sulfuric acid micro-assay of Wang et al.
(2016). Protein content was determined by the Bradford method. Dif-
ferent concentrations of BSA were used to obtain a calibration curve.
Samples were tested in triplicates.
2.5.4. High-performance size exclusion chromatography (HPSEC)
The molecular weight distribution of the target products was as-
sessed by HPSEC (Li, Xia, Nie, & Shan, 2016). The instruments consisted
of an Agilent 1100 chromatographic instrument and a Shodex OHPak
SB-804HQ (8 mm ID × 300 mm L), operating at 35 °C with a RID-10A
detector (SHIMADZU). The mobile phase was phosphate buffer
(0.0177 M NaH2PO3, 0.0079 M Na2HPO3, flow rate, 0.5 mL/min).
Shodex Standard P-82 Pullulan (Mw 6.2, 10.0, 21.7, 48.8, 113, and
210 kDa) was used as the calibration standard.
2.5.5. Fourier transform infrared spectroscopy (FTIR) analysis
The FTIR spectra of pectin were obtained at a resolution of 4 cm−1.
The effects of microwave power levels (160, 240, 320, 400, and
480 W) on PY are summarized in Fig. A1 (supplementary material)).
With the other factors fixed (pH 1.0, LSR 25, and 6 min irradiation), PY
significantly increased from 4.1% to 26.1% as the power increased from
160 to 400 W. In a previous study, PY increased with increasing mi-
crowave power levels (Hosseini, Khodaiyan, & Yarmand, 2016a,
2016b). Fig. A1 shows that PY decreased at > 400 W, which could be
due to pectin degradation. Therefore, microwave power was set at
400 W for all subsequent extraction procedures.
3.1. Statistical analysis
BBD for the three variables in three levels and three replications was
applied to optimize PY. The experimental results and predicted values
for all variables are shown in Table 1. ANOVA results revealed that the
effects of linear and quadratic terms on PY and GA content were ex-
tremely significant (p < 0.01; Table 2). Similarly, the quadratic term
on DE was extremely significant, and the linear term on DE was sig-
nificant (p < 0.05). The quadratic polynomial regression was well

3
D.-L. Su, et al. Food Chemistry 286 (2019) 1–7

Table 2 required for pectin exposure to the release medium, pectin dissolution,
Analysis of variance (ANOVA) for PY, GA content, and DE of orange peel pectin. and pectin diffusion from the raw solid materials (Samavati, 2013).
Source Sum of squares DF Mean square F-Value p-Value LSR and pH were two other factors that affected PY. As shown in
Fig. 1b and c, PY significantly increased up to 24.9 LSR. Very high LSR
(A) PY values decreased PY. Maran, Sivakumar, Thirugnanasambandham, and
Model 96.65 9 10.74 21.27 0.0003
Sridhar (2014) postulated that the solvent could efficiently absorb
Linear 77.64 3 25.88 14.93 0.0002
2FI 4.63 3 1.54 0.86 0.4919
microwave energy and promote swelling of plant material; however,
Quadratic 14.37 3 4.79 9.49 0.0073 higher volumes of solvent could potential decrease the microwave ad-
Residual 3.53 7 0.50 sorption of material. Fig. 1a and b shows that PY increased as pH de-
Lack of Fit 1.20 3 0.40 0.69 0.6052 creased from 1.5 to 1.0. The low acid extraction solvent had the ability
Pure Error 2.33 4 0.58
to contact the insoluble pectin directly and favored the hydrolysis of the
Cor Total 100.18 16
2 2 2
R = 0.9647, Adj R = 0.9194, and Pred R = 0.7716 insoluble pectin constituents into soluble pectin, thereby increasing PY
(Maran, Sivakumar, Thirugnanasambandham, & Sridhar, 2013). How-
(B) GA
Model 2396.71 9 266.30 33.75 < 0.0001 ever, pectin aggregation occurred at pH < 1.0, which decreased pectin
Linear 2140.81 3 713.60 29.82 < 0.0001 release and PY.
2FI 21.40 3 7.13 0.25 0.8622
Quadratic 234.50 3 78.17 9.91 0.0065 3.3. Effect of processing variables on GA content of pectin
Residual 55.24 7 7.89
Lack of Fit 17.73 3 5.91 0.63 0.6329
Pure Error 37.51 4 9.38 Table 1 shows that GA ranged from 23.4% (run No. 3) to 63.5% (run
Cor Total 2451.95 16 No. 17). ANOVA results and Eq. (8) indicated that pH had the greatest
R2 = 0.9775, Adj R2 = 0.9485, and Pred R2 = 0.8604 effect on GA content. Fig. 1d and e shows that high pH values favored
(C) DE the production of pectin with high GA content. To the best of our
Model 2286.90 9 254.10 52.19 < 0.0001 knowledge, no studies have evaluated the effect of pH on the GA con-
Linear 1029.52 3 343.17 3.45 0.0483 tent of pectin. Harsh extraction conditions (pH < 1.0) may increase
2FI 467.02 3 155.67 1.89 0.1955
Quadratic 790.37 3 263.46 54.11 < 0.0001
de-polymerization of polysaccharides, such as cellulose and hemi-
Residual 34.08 7 4.87 cellulose, which contribute to the release of water-soluble pectin from
Lack of Fit 28.13 3 9.38 6.30 0.0537 plant tissue. The effects of irradiation time and LSR were negligible
Pure Error 5.95 4 1.49 compared to pH. Fig. 1d and f shows that GA content increased with
Cor Total 2320.98 16
2 2 2 increasing irradiation time, as previously reported (Bagherian et al.,
R = 0.9853, Adj R = 0.9664, and Pred R = 0.8021
2011).

fitted to the experimental data, because the lack-of-fit test was insig-
nificant for each of the three parameters at 0.6052, 0.6329, and 0.0537.
Only 3.53%, 2.25%, and 1.47% of the data were not explained by the
model (R2 = 96.47, 97.75, and 98.53%, respectively). Moreover, the
values of the adjusted determination coefficient (adjusted
R2 = 91.94%, 94.85%, and 96.64%, respectively) revealed that the
model was adequate (Hosseini, Khodaiyan, & Yarmand, 2016a, 2016b).
Our findings suggested that the second-order equation was sufficient to
predict the effects of the three independent variables. The second-order
equations related to PY (Eq. (7)), GA content (Eq. (8)), and DE (Eq. (9))
for achieving maximum yield were expressed as follows,
3.4. Effect of processing variables on DE of pectin
As shown in Table 1, pectin DE ranged from 31.7 (run No. 14) to
72.8% (run No. 9). At high pH, moderate irradiation time and LSR fa-
vored the formation of pectin with high DE. The results were in ac-
cordance with previous studies (Hosseini, Khodaiyan, & Yarmand,
2016a, 2016b; Jafari et al., 2017). In general, pectin obtained under
very harsh extraction conditions (high power, long irradiation time,
and low pH) have low DE, because these harsh conditions promote the
de-esterification of polygalacturonic chains (Wai, Alkarkhi, & Easa,
2010).

PY (%) = 27.36 + 0.71X1 + 2.90X2 − 0.89X3 − 0.30X1 X2 − 0.88X1 X3
− 0.55X2 X3 − 1.24X12 + 0.28X22 − 1.29X32
GA (%) = 50.78 + 16.23X1 + 1.89X2 − 0.89X3 + 1.47X1 X2 + 1.48X1 X3
− 1.00X2 X3 − 7.24X12 + 2.08X22 − 0.31X32
DE (%) = 70.86 + 10.29X1 + 4.33X2 − 2.04X3 − 9.53X1 X2 +2.45X1 X3
− 4.48X2 X3 − 6.91X12 −9.08X22 − 6.20X32
3.2. Effect of processing variables on PY
Table 1 shows that PY ranged between 22.3 (run No. 14) and 30.3%
(run No. 12). The optimum conditions for these factors were obtained
by solving models of Eq. (7). The parameter optimization modeling
suggested that the optimum conditions were pH 1.2, 7.0 min irradia-
tion, and 21.5 LSR. Under these conditions, PY was 31.1% as expected
from BBD. Validation experiments showed that the highest PY obtained
was 28.0 ± 0.5%, which indicated that there was a high degree of fit
between the values observed in the experiments and the values pre-
dicted by the model. ANOVA results and Eq. (7) revealed that the
greatest effect on PY was irradiation time. Fig. 1a and c shows that a
longer irradiation time favored PY. This result might be due to the time
3.5. Extraction of pectin from dried orange peels using S-MAE
(7)
The optimized microwave extraction conditions (pH 1.2, 7.0 min
irradiation, and 21.5 LSR) and microwave power (400 W) were kept
(8) constant. The effects of different surfactants (Tween-80, Tween-20, PEG
4000, PEG 8000, SE, and SDS) on PY are shown in Fig. 2. Among the
surfactants, PEG 4000 had a slight effect on PY, while SE negatively
affected PY. PY decreased when the concentration of SDS increased
(9)
from 2 to 8 g/L; however, PY increased as the concentration increased
to 10 g/L SDS. This finding was not consistent with a past study, which
reported that SDS (8 g/L, w/v) increased PY during MAE (Hui-jin, Fang-
yan, LI-guo, & Shuai, 2014). Our findings revealed that PEG 8000,
Tween-20, and Tween-80 increased PY significantly (p < 0.05). When
the concentration of Tween-80 increased to 8 g/L (w/v), PY increased
by 17.0% compared to the control. Tween-80, a non-ionic surfactant,
had a higher extraction efficiency than SDS, an ionic surfactant.
Hosseinzadeh, Khorsandi, and Hemmaty (2013), who studied the ef-
fects of surfactants on polyphenolic compounds extracted from apples,
concluded that non-ionic surfactants had better extraction efficiency
than ionic types. The effect of surfactant structure on the extraction of
polyphenolics is dependent on the balance between hydrophobic and
hydrophilic forces. Ionic surfactants make ion-pairs with ionic phe-
nolics and induce turbidity in solutions; therefore, extraction

4
D.-L. Su, et al. Food Chemistry 286 (2019) 1–7

Fig. 1. Effect of processing variables on pectin yield (PY; a, b, and c), GA content (d, e, and f), and DE (g, h, and i).

percentage is lower for ionic surfactants than for non-ionic surfactants.

3.6. Comparison of extracted pectin using MAE, S-MAE, and CE methods

We compared pectin extraction from OPP by different extraction

Fig. 2. Relative pectin yield by microwave (MAE) and surfactant- microwave
assisted extraction (S-MAE). Control is microwave extraction without surfactant
added.
methods including the CE, MAE, and S-MAE (Table 3). Pectin DE varied
from 61.0% to 71.3%, which fell in the range of “commercially avail-
able food-grade high methoxyl pectin.” GA content ranged from 68.2%
to 78.1%, which is favorable in food industry applications (Bagherian
et al., 2011). Total sugar content varied from 78.2% to 84.2%, in
agreement with grapefruit peel pectin extracted by UAE (M. Wang
et al., 2016). Compared to the CE method, the S-MAE method resulted
in pectin with significantly (p < 0.05) higher PY (32.8%), GA content
(78.1%), DE (69.8%), Mw (286.3 kDa), and total sugar content (84.2%).
In addition, S-MAE resulted in a lower protein content (p < 0.05;
5.8%) than CE. The results revealed that S-MAE offered several ad-
vantages, such as higher extraction efficiency and better product
quality.
Fig. 3a and Table 3 show that the Mw value of OPP pectin isolated by
optimal microwave conditions was 144.8 kDa, in accordance with a
previous finding (Kostalova et al., 2016). In this study, the Mw of pectin
extracted by S-MAE (286.3 kDa) was higher (p < 0.05) than that ex-
tracted by CE or MAE (Table 3). It is possible that the presence of
Tween-80 favored pectin extraction and maintained the structure of the
macromolecule. Additionally, microwave-assisted processes require
shorter processing times than the CE method, thereby reducing energy
costs (Seixas et al., 2014). The conventional process lasted 3 h, while

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D.-L. Su, et al. Food Chemistry 286 (2019) 1–7

Table 3
The qualitative and quantitative characteristics of extracted pectin from different methods.
Pectin* Properties
PY (%) GA (%) DE (%) Mw (kDa) Total sugar content (%) Protein content (%)

CP − 64.4 ± 1.2a 63.3 ± 0.5a 146.7 ± 3.5a 78.2 ± 1.5a 4.7 ± 0.3a
CE 27.5 ± 0.6a 68.3 ± 2.1a 61.0 ± 0.8b 137.1 ± 3.0b 77.2 ± 1.0a 7.1 ± 0.6b
MAE 28.0 ± 0.5a 68.2 ± 2.4a 71.3 ± 0.6c 144.8 ± 2.0ab 80.2 ± 0.5a 7.0 ± 0.2b
S − MAE 32.8 ± 0.8b 78.1 ± 2.0b 69.8 ± 0.4c 286.3 ± 5.2c 84.2 ± 2.1b 5.8 ± 0.5a

* CP: commodity pectin; CE: conventional extraction; MAE: microwave assisted extraction; S-MAE: Surfactant and microwave assisted extraction. Values with
different letters (a, b, and c) are significantly different (p < 0.05); n = 3.

bands at 1643 and 1446 cm−1 were attributed to asymmetric and

symmetric stretching modes of the COO− group, and the characteristic
absorptions at 825 and 930 cm−1 in the IR spectra indicated that α- and
β-configurations were simultaneously present in pectin (Li et al., 2016).

3.8. SEM analysis of extracted residues

Fig. A2 (supplementary material) shows the SEM images of OPP

before and after extraction. The structure of the untreated peel sample
remained smooth and compact (Fig. A2a), but it showed signs of de-
composition following CE (Fig. A2b). After MAE or S-MAE, the original
structure was destroyed and became lose (Fig. A2c and d). This finding
revealed that microwave irradiation significantly damaged the micro-
structure of the peels to facilitate extraction of the pectin, which was in
agreement with our previous report (Li, Xia, Shan, Nie, & Wang, 2015).
The mechanism of microstructure destruction could be due to the rapid
increase of temperature in the cells of the peels, which increased in-
tracellular pressure. When the pressure exceeds a critical limit, the cell
wall is rapidly ruptured facilitating the release of pectin to the extrac-
tion media.

4. Conclusions

In this study, we used S-MAE to extract pectin from OPP. First, the
microwave extraction conditions were optimized for pectin extraction.
The highest PY (28.0 ± 0.5%, which was close to the predicted value
of 31.1%) was obtained at 400 W, pH 1.2, 7.0 min irradiation, and 21.5
(mL/g) LSR. Furthermore, under the optimal microwave conditions and
in the presence of Tween-80 (8 g/L, w/v), PY increased by 17.0%
compared with MAE. Overall, S-MAE was a useful alternative to the
conventional extraction method, which offered several advantages such
as reduced extraction time, higher yield, higher pectin quality, and
lower energy costs.

Fig. 3. HPSEC chromatograms (a) and FTIR (b) of pectin from CP, CE, MAE, Conflict of interest
and S-MAE (CP: commodity pectin; CE: conventional extraction; MAE: micro-
wave-assisted extraction; S-MAE: surfactant-microwave assisted extraction). The authors declare that there is no conflict of interest.

the microwave process required 7 min to achieve the same yield. Acknowledgements

3.7. FTIR analysis of pectin
The infrared spectra of pectin extracted by different methods are
shown in Fig. 3b. The peaks at approximately 3429 and 2928 cm−1
corresponded, respectively, to stretching vibrations of hydroxyl groups
(OH) and CeH of CH, CH2, and CH3 groups. DE values depended on the
absorbance intensity ratio between the band at 1745 cm−1 and the sum
of the bands at 1745 and 1608 cm−1 (Zainudin, Wong, & Hamdan,
2018). The DE values of pectin extracted by CE, MAE, and S-MAE were
54.8, 64.5, and 73.3%, respectively (Fig. 3b). The difference in DE
values obtained from the chemical method (Table 3) and FTIR was
attributed to the presence of impurity residues in pectin. A couple of
This study was financially supported by a grant from the Innovative
Platform and Talent Plan of Hunan Province (Project No. 2016RS2018),
the One hundred Talents Project of Hunan Province (2016 Year), the
Innovative Team of Agricultural Science and Technology Innovative
Fund of Hunan Province (Project No. 2017GC03), Research Program of
Guangxi Specially-invited Experts (Key Technologies for Intensive
Processing and Quality Safety of Agricultural Products, Ting Fa [2018]
39th), and the Scientific-Technological Platform of Innovation and
Starting Businesses Plan of Hu-xiang Youth Training Objects (Project
No. Xiang Ke Ren Zi [2014] 76th). We thank International Science
Editing (http://www.internationalscienceediting.com) for editing this
manuscript.

6
D.-L. Su, et al.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.foodchem.2019.01.200.
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