Innovative Food Science and Emerging Technologies 74 (2021) 102850

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Innovative Food Science and Emerging Technologies

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Single-step recovery of pectin and essential oil from lemon waste by ohmic
heating assisted extraction/hydrodistillation: A multi-response
optimization study
Merve Tuğçe Tunç , Halil İbrahim Odabaş *
Gümüşhane University, Faculty of Engineering and Natural Sciences, Department of Food Engineering, Gümüşhane, Turkey

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

Keywords: The main products obtained from citrus wastes are pectin and essential oil. In this work, ohmic heating assisted
Ohmic heating extraction/hydrodistillation (OHAE/H) was applied for the simultaneous recovery of pectin and essential oil
Extraction from lemon waste. Optimum OHAE/H conditions to maximize the yield of pectin and essential oil were deter­
Hydrodistillation
mined with response surface methodology. Three independent variables, namely liquid to solid ratio (w:v),
Pectin
Essential oil
extraction/hydrodistillation time (min) and voltage gradient (V/cm) were varied to obtain maximum pectin and
essential oil yield. Optimum OHAE/H conditions were determined as 8.7:1 liquid to solid ratio, 58.4 min
extraction/hydrodistillation time and 14.2 V/cm voltage gradient. The predicted pectin and essential oil yields at
optimum conditions were 16.58 and 3.62 g/100 g lemon waste, respectively. Data analysis showed that all of the
independent variables significantly affected the pectin and essential oil yield. In the verification study, close
agreement was found between predicted and experimental values. Conventional heating extraction/hydro­
distillation (CHE/H) were conducted to evaluate the effectivity of OHAE/H. With OHAE/H process, the yields of
the pectin and essential oil were significantly increased when compared to CHE/H. Limonene concentration of
the essential oil produced with OHAE/H was higher than the essential oil produced by CHE/H. Results
demonstrate that the single-step OHAE/H could be an effective method for simultaneous extraction and
hydrodistillation of pectin and essential oils.

1. Introduction and stabilizer (Dimopoulou, Alba, Campbell, & Kontogiorgos, 2019).

Wastes of the food processing industry exhibit environmental and
economic problems due to their high quantities of over 1.3 billion tonnes
per year (Patsalou, Chrysargyris, Tzortzakis, & Koutinas, 2020). Fruit
processing plays an important role in the waste generation (El-Gengaihi
et al., 2020). The amount of citrus fruits that produce 124 million tons
annually exceeds 25 million tons is citrus peel waste, globally (Patsalou
et al., 2020). Citrus wastes have economic potential for industry because
of important components such as pectin, essential oil, polyphenols, ca­
rotenoids and vitamins (Costa, Albergamo, Arrigo, Gentile, & Dugo,
2019). Thus, finding novel energy-efficient and economic strategies to
valorize the citrus waste to produce value-added products is essential for
the food processing industry.
Pectin and essential oil are two main value-added products obtained
from lemon waste (John, Muthukumar, & Arunagiri, 2017). Pectin has
excellent features such as dietary fibre, thickener, emulsifier, texturizer
Essential oils are volatile and aromatic products which obtained from
aromatic plants, herbs and spices and they have been used in food,
cosmetic and pharmaceutical industry due to their aroma, antioxidant,
anticancer, antimicrobial and anti-inflammatory properties (Hasani,
Ojagh, & Ghorbani, 2018; Ribeiro-Santos, Andrade, Sanches-Silva, & de
Melo, 2018).
Pectin is conventionally produced by acidic water extraction (Marić
et al., 2018). Major drawbacks of the conventional method are the long
extraction times and degradation of the pectin during extraction
(Bagherian, Zokaee Ashtiani, Fouladitajar, & Mohtashamy, 2011).
Recently alternative green technologies have been introduced for
extraction of pectin such as ultrasound-assisted extraction (Khedmat,
Izadi, Mofid, & Mojtahedi, 2020), microwave-assisted extraction (Kar­
buz & Tugrul, 2020) and enzyme assisted extraction (Picot-Allain,
Ramasawmy, & Emmambux, 2020). Conventional methods for extract­
ing the essential oils from citrus wastes are steam distillation,

* Corresponding author at: Department of Food Engineering, Faculty of Engineering and Natural Sciences, Gümüşhane University, 29100 Gümüşhane, Turkey.
E-mail address: hiodabas@gumushane.edu.tr (H.İ. Odabaş).

https://doi.org/10.1016/j.ifset.2021.102850
Received 10 February 2021; Received in revised form 1 August 2021; Accepted 4 October 2021
Available online 6 October 2021
1466-8564/© 2021 Elsevier Ltd. All rights reserved.
M.T. Tunç and H.İ. Odabaş
Fig. 1. Schematic diagram of the OHAE/H system.
hydrodistillation and cold pressing (Ferhat, Meklati, & Chemat, 2007).
Ultrasound-assisted hydrodistillation (Cebi et al., 2019), microwave-
assisted hydrodistillation (Kapadiya, Parikh, & Desai, 2018), supercrit­
ical fluid extraction (Pokrovskiy et al., 2019) methods were used for
recovery of the essential oils.
Reducing energy and cost in industry is very important to future
world because of inadequate energy sources, environmental and eco­
nomic problems (Bozkurt & Içier, 2012). Ohmic heating has potential to
be used for different applications such as blanching (Icier, Yildiz, &
Baysal, 2006), pasteurization (Silva et al., 2020), evaporation (Darvishi,
Hosainpour, Nargesi, & Fadavi, 2015) and thawing (Roberts, Balaban,
Zimmerman, & Luzuriaga, 1998) due to its lower energy consumption
and higher heating rate compared to conventional heating methods.
Besides its rapid heating rate, electrical field result in the electroporation
of the cell membranes and improves the extraction yield (Chemat et al.,
2020). Ohmic heating assisted extraction could be classified as a green
technology with its rapid heating rate, higher extraction yield, higher
extract quality and, lower energy consumption and time (M. Gavahian,
Lee, & Chu, 2018; Hashemi, Kamani, Amani, & Mousavi Khaneghah,
2019). Ohmic heating assisted hydrodistillation of essential oils from
different vegetal tissues were successfully applied by different research
groups (Hashemi et al., 2019; Taban, Saharkhiz, & Niakousari, 2018;
Tunç & Koca, 2019). Recently, there have been some attempts to use of
ohmic heating for extraction of pectin from tomato processing waste
(Sengar, Rawson, Muthiah, & Kalakandan, 2020), orange juice waste
(Saberian, Hamidi-Esfahani, Ahmadi Gavlighi and Barzegar, 2017) and
lemon peel powder (Çilingir, Goksu, & Sabanci, 2021).
Since the natural sources was decreased, it is very important to
maximize the amount of valorizable products from by-products or
wastes of food industry (Chemat et al., 2019). Simultaneous extraction
of multiple value-added products with a single-step process could be an
innovative strategy to reduce production costs and environmental im­
pacts and has gained a lot of attention. Recently, few authors have
attempted to extraction of multiple products with a single process.
Several studies have focused on the simultaneous extraction of pectin
and phenolic compounds from different biological materials such as sour
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Innovative Food Science and Emerging Technologies 74 (2021) 102850
cherry pomace (Hosseini, Parastouei, & Khodaiyan, 2020), black mul­
berry pomace (Khodaiyan & Parastouei, 2020), pomegranate peels
(Talekar, Patti, Vijayraghavan, & Arora, 2018) and mango peels (Rojas
et al., 2020). Some studies have also attempted to combine the extrac­
tion and hydrodistillation processes for single-step production of pectin
and essential oils. Tuan, Dang, Huong, and Danh (2019) were combined
the extraction and hydrodistillation processes to produce pectin and
essential oil from pomelo peel by one-step extraction/hydrodistillation
process. Fidalgo et al. (2016), simultaneously extracted pectin and
essential oil from lemon and orange waste by microwave assisted
extraction/hydrodistillation.
There are no studies in the literature about co-extraction of pectin
and essential oils by ohmic heating to the best of our knowledge. Thus,
the objective of this study was (1) the determination of the effects of
OHAE/H variables (voltage gradient, extraction/hydrodistillation time,
and liquid to solid ratio) on the yield of essential oil and pectin, (2) the
optimization of the single step production process of two main value-
added products (essential oil and pectin) of lemon waste with OHAE/
H, (3) the comparison of the OHAE/H and CHE/H methods in terms of
pectin yield, essential oil yield, pectin properties and essential oil
composition.
2. Material and methods
2.1. Materials
Fresh lemons (Citrus limon) were purchased from a local store in
Gümüşhane, Turkey. They were squeezed with a manual citrus press.
The lemon waste was then blanched for 3 min to inactivate the enzymes
and were stored in polyethylene bags at − 18 ◦ C during the experiments.
All chemicals and reagents were of analytical grade.
2.2. Methods
2.2.1. Ohmic heating assisted extraction/hydrodistillation (OHAE/H)
OHAE/H experiments were performed in a ohmic heating system
M.T. Tunç and H.İ. Odabaş Innovative Food Science and Emerging Technologies 74 (2021) 102850

Table 1 extracted pectin samples by OHAE/H and CHE/H were conducted using
Central composite design and experimental pectin and essential oil yield results. a rheometer (Anton Paar MCR 102, Thermo Scientific, Germany)
Run LSr E/H time VG Pectin yield Essential oil yield equipped with a parallel plate (diameter 35 mm, gap 1.000 mm). One
gram of the pectin sample was dissolved in 100 mL of distilled water.
(w:w) (min) (V/cm) (g/100 g dw) (g/100 g dw)
Then, the sample was placed between a parallel-plate using a gap size of
1 5 30 15 9.27 2.22 1 mm. The flow experiments were conducted under steady-shear con­
2 15 30 15 14.69 1.63
3 5 60 15 13.58 3.52
ditions with shear rate ranging from 1 to 100 s− 1 at 25 ◦ C. The flow
4 15 60 15 16.54 2.22 behavior of pectin solutions was analyzed by using Power law model
5 5 45 10 9.81 2.82 based on the following equation:
6 15 45 10 15.47 2.44
7 5 45 20 9.6 3.79 τ = K.γ˙n (3)
8 15 45 20 12.43 2.28
9 10 30 10 13.71 1.73 where τ is the shear stress (mPa), γ ˙ is the shear rate (s− 1), K is the
10 10 60 10 16.58 3.58
consistency coefficient (mPasn), and n is the flow behavior index
11 10 30 20 11 2.82
12 10 60 20 14.36 3.41 (dimensionless).
13 10 45 15 15.84 3.3 The frequency sweep test was done a fixed strain of 0.5%. The
14 10 45 15 14.98 3.58 OHAE/H and CHE/H solutions were rested on the plate during 5 min for
15 10 45 15 15.51 3.2 relaxation before oscillatory tests. Frequency sweep experiments were
16 10 45 15 16.33 3.41
performed between 0.1 and 100 Hz within Linear Viscoelastic Range
17 10 45 15 15.76 3.41
(LVR) at 25 ◦ C. Temperature sweeps were carried out from 4 ◦ C to 90 ◦ C
with heating rate of 0.05 ◦ C/s at the constant 0.5% shear strain, within
with titanium electrodes as described in the study by Tunç and Koca LVR. Oscillatory measurements were used to determine the storage
(2019). A schematic diagram of the OHAE/H system was shown in modulus (G′ ), loss modulus (G′′ ), and tangent delta (tan δ = G′′ /G′ )
Fig. 1. A predetermined amount of lemon waste (varied according to the values of the samples.
liquid to solid ratio) and 250 mL of citric acid solution (pH 2) were
transferred to the ohmic heating cell. System was worked with different 2.2.3.3. Infrared spectral analysis. Fourier Transform Infrared (FTIR)
voltage gradients and extraction/hydrodistillation times. The experi­ spectra of the pectin samples were recorded in the range of 4000 and
mental design and corresponding pectin and essential oil yields were 600 cm− 1 with a resolution range of 4 cm− 1 by a FTIR spectrophotom­
shown in Table 1. The levels of the independent variables were deter­ eter (Spectrum Two, Perkin Elmer).
mined with preliminary experiments (data not shown). After the
extraction/hydrodistillation, essential oil in the Clevenger apparatus 2.2.3.4. Thermal properties. A differential scanning calorimeter (DSC
was collected in an amber colored vial, dried over anhydrous sodium 4000, Perkin Elmer) was used for the investigation of the thermal
sulfate, and weighed. While, pectin-rich solution in the ohmic heating properties of pectin samples. Analysis conditions were as follows:
cell was immediately cooled to room temperature and vacuum filtered. 40–300 ◦ C tempreture range, 10 ◦ C/min heating rate, 20 mL/min ni­
Pectin was precipitated with 2-fold volume of 96% ethanol (v:v). trogen purge. 5 mg of pectin sample was placed in an aluminum pan.
Precipitated pectin was washed with 96% ethanol (v:v) twice and dried Empty pan was used as reference.
in a laboratory oven at 45 ◦ C until a constant weight. Pectin and
essential oil yields were calculated with following equation: 2.2.3.5. Scanning electron microscopy. Particle morphologies of the
Weight of dried pectin or essential oil pectin samples were evaluated using a scanning electron microscobe
Yield (g/100g) = × 100 (1) (JSM-7001F, Jeol). Samples were coated with gold‑palladium alloy
Dry weight of the lemon peel
under vacuum before analysis. The scanning electron microscope was
Total consumed energy (J) was calculated using following equation used at 5 kV and magnified to ×100, ×500, ×1000 and ×3000.
described in Silva et al. (2020);
∑ 2.2.4. Chemical composition of essential oil
E= (VIt) (2)
Lemon essential oils were analyzed by GC (Agilent GC 7890A)
where E; electrical energy consumption, V; applied voltage, I; electrical coupled with MSD detector (Agilent 5975C VL). The column was HP-
current, t; time interval. 5MS (30 m length, 0.25 mm diameter and 0.25 μm film thickness).
Helium (1 mL/min of flow rate) was used as a carrier gas. The injection
2.2.2. Conventional heating extraction/hydrodistillation (CHE/H) and detection temperatures were set at 250 ◦ C. The temperature of the
About 28.60 g of lemon waste was weighed in a flat bottom flask oven was gradually increased from 45 ◦ C to 230 ◦ C with heating rate of
connected to a Clevenger apparatus and extracted/hydrodistilled with 3 ◦ C/min. Appropriately diluted essential oil samples (with methanol)
250 mL of citric acid solution (pH 2). Total extraction/hydrodistillation were injected into the GC/MS with split mode. The compounds of lemon
time was 58.35 min. The mixture was heated with a magnetic stirrer/hot essential oil were identified by matching their mass spectra with those of
plate. After the extraction/hydrodistillation, same procedure with pure compounds.
OHAE/H was followed. Total consumed electrical energy was measured
using a watt-meter (TT T-ECHNI-C, China). 2.2.5. Experimental design and statistical analysis
A Box-Behnken Design based on response surface methodology with
2.2.3. Characterization of pectin three factors (liquid to solid ratio, extraction/hydrodistillation time and
voltage gradient) at three levels was employed to optimization and the
investigation of the effects of OHAE/H variables on pectin and essential
2.2.3.1. Degree of esterification and galacturonic acid content. The degree
oil yield. Planning to experimental design, statistical analysis, fitting the
of esterification and galacturonic acid contents of the lemon waste
model and determination of the optimum OHAE/H conditions were
pectin samples extracted by OHAE/H and CHE/H were analyzed with
done using the software Minitab (Version 18.0, Minitab Inc., USA). The
the method described by FAO/WHO (2007).
significance of the OHAE/H variables and their interactions were eval­
uated using ANOVA. Fisher’s test was used for the determination of the
2.2.3.2. Rheological properties. Rheological measurements of the
significance of the models and regression coefficients. The adequacy of

3
M.T. Tunç and H.İ. Odabaş Innovative Food Science and Emerging Technologies 74 (2021) 102850

Table 2
ANOVA for the fitted models.
Source SS DF MS F-value p-value

PY EOY PY EOY PY EOY PY EOY PY EOY

Model 4.92 7.53 9 9 0.55 0.84 58.44 48.82 < 0.0001 < 0.0001
A 1.75 1.79 1 1 1.75 1.79 186.49 104.25 < 0.0001 < 0.0001
B 0.94 2.34 1 1 0.94 2.34 100.69 136.80 < 0.0001 < 0.0001
C 0.41 0.37 1 1 0.41 0.37 43.72 21.84 0.0003 0.0023
AB 0.07 0.13 1 1 0.07 0.13 7.95 7.36 0.0258 0.0301
AC 0.10 0.32 1 1 0.10 0.32 10.51 18.63 0.0142 0.0035
BC 0.00 0.40 1 1 0.00 0.40 0.32 23.17 0.5904 0.0019
A2 0.93 1.13 1 1 0.93 1.13 99.50 65.82 < 0.0001 < 0.0001
B2 0.00 0.91 1 1 0.00 0.91 0.035 53.14 0.8562 0.0002
C2 0.62 0.00 1 1 0.62 0.00 66.31 0.22 < 0.0001 0.6524
Residual 0.07 0.12 7 7 0.01 0.02
Lack of Fit 0.02 0.04 3 3 0.01 0.01 0.49 0.65 0.7101 0.6229
Pure Error 0.05 0.08 4 4 0.01 0.02
Cor Total 4.99 7.65 16 16

SS: sum of squares, MS: mean squares, PY: pectin yield, EOY: essential oil yield.

the models for pectin and essential oil yield were checked using coeffi­
cient of variation (CV), coefficients of determination (R2, adjective R2
and predicted R2) and lack of fit test. The optimum OHAE/H conditions
that maximize the pectin and essential oil yield was determined by
desirability function. Validation of the optimum OHAE/H conditions
were done by comparison of the predicted and the experimental pectin
and essential oil yield.
The differences between the properties of pectin and essential oil
samples extracted by OHAE/H and CHE/H were evaluated by Student’s
t-test at a 95% confidence level using the SPSS software (Version 22.0,
IBM, USA).
3. Results and discussion
3.1. Model fitting
The design matrix and the corresponding pectin and essential oil
yield results of the RSM experiment are shown in Table 1. As shown in
Table 1, pectin and essential oil yields ranged from 9.27 to 16.58% and,
from 1.63 to 3.89%, respectively. Our results were in agreement with the
data reported by other authors. Masmoudi et al. (2008), found that the
yield of lemon peel pectin extracted by acidified date juice at optimum
extraction conditions was 11.21%. Martínez-Abad et al., 2020, reported

Fig. 2. Pareto charts and normal plots of the standardized effects of OHAE/H variables on pectin (A1 and A2) and essential oil yield (B1 and B2).

4
M.T. Tunç and H.İ. Odabaş
Fig. 3. Three dimensional response surface graphs and contour plots for pectin yield.
that the lemon essential oil yield was 2.03% with microwave assisted
hydrodistillation. It is crucial to remember that the yields of pectin and
essential oil depending on the agricultural practices, cultivar charac­
teristics and extraction methods.
A regression analysis was made to fit mathematical models to the
experimental data. Predicted response for the pectin (Yp) and essential
oil (Yeo) yields could be expressed by the following equations which are
empirical relationships between pectin and essential oil yield and the
OHAE/H variables in actual units.
Yp = − 21.386 + 2.914 X1 + 0.177 X2 + 2.083 X3 − 0.008 X1 X2 − 0.028X1 X3
+ 0.002 X2 X3 − 0.084 X12 − 0.000 X22 − 0.069 X32
Yeo = − 10.068+0.596 X1 +0.309 X2 +0.381 X3 − 0.002 X1 X2 − 0.011 X1 X3
+0.004 X2 X3 − 0.021 X12 − 0.002 X22 − 0.001 X32
where, Yp and Yeo is the yields of pectin and essential oil, respectively
and, X1, X2 and X3 are the actual variables for liquid to solid ratio,
extraction/hydrodistillation time and voltage gradient, respectively.
The results of ANOVA are presented in Table 2. The small p-values
(<0.0001) suggested that the regressions models for pectin yield and
essential oil yield were significant. The non-significant lack of fit values
for both of the models at 95% confidence level indicates that the models
adequately represented the data. The coefficients of determination (R2)
were 0.9869 and 0.9843 for the models described the pectin yield and
essential oil yield, respectively. The high R2 values suggested that the
high degree of correlation between experimental and predicted pectin
and essential oil yields. The agreement between the adj.R2 and pred.R2
values indicated reliabilities of the models were good. Low coefficient of
variation (CV) values of 3.15 and 4.51 indicated that the reproducibility
of the models for pectin yield and essential oil yield, respectively, was
high.
3.2. Effects of the OHAE/H variables on the pectin yield
Table 2 shows the results of ANOVA for each independent variable
Innovative Food Science and Emerging Technologies 74 (2021) 102850
and their interactions for the pectin yield. As presented in Table 2, linear
effects of the all independent variables were significant on the pectin
yield. The effects of the interactions of liquid to solid ratio-extraction/
hydrodistillation time and liquid to solid ratio-voltage gradient were
significant, while the effect of the interaction term of extraction/
hydrodistillation time-voltage gradient was not significant. The
quadratic terms have significant effect on pectin yield except the
quadratic term of extraction/hydrodistillation time.
F values from the ANOVA table, Pareto chart (Fig. 2A.1) and the
normal plot of the standardized effects (Fig. 2A.2) show the magnitudes
the effects of the independent variables on pectin yield during OHAE/H.
From the ANOVA table and Pareto chart, it was concluded that the most
(4) significant linear variable was the liquid to solid ratio (F-value 186.49)
followed by extraction/hydrodistillation time (F-value 100.69) and
voltage gradient (F-value 43.72). The most effective interaction and
quadratic terms on pectin yield was liquid to solid ratio-voltage gradient
(5) (F-value 10.51) and liquid to solid ratio*liquid to solid ratio (F-value
99.5), respectively. The effects of the liqud to solid ratio and extraction/
hydrodistillation time showed a synergistic effect for the pectin yield.
However, all of the significant interaction and quadratic terms with the
voltage gradient showed an unfavorable effect for pectin yield
(Fig. 2A.2).
Three dimensional response surface graphs (Fig. 3A), contour plots
(Fig. 3B) show the effects of OHAE/H variables on pectin yield during
OHAE/H process. As shown, the pectin yield increased gradually as the
liquid to solid ratio increased from 5:1 to 12:1. However, when the
liquid to solid ratio continued to increase, the pectin yield slightly
decreased. The lower pectin yield at lower liquid to solid ratios may be
due to the insufficient amount of the extraction solution required for
solubilizing the pectin (Kulkarni & Vijayanand, 2010). Increasing pectin
yield as a result of the increasing liquid to solid ratio from 5:1 to 12:1 is
probably due to the enhance the diffusion of the solvent into solid ma­
terial (Ke et al., 2020). Furthermore, at relatively high liquid to solid
ratios may cause the excessive swelling of the plant material and this
may increase the absorbed electrical energy. However, at higher liquid
to solid ratios than 12:1, limited amount of extracted pectin may un­
dergo degradation possibly due to the excessive heating.
As shown in the Fig. 3A and Fig. 3B, pectin yield was increased with
5
M.T. Tunç and H.İ. Odabaş
Fig. 4. Three dimensional response surface graphs and contour plots for essential oil yield.
the increasing extraction/hydrodistillation time. Similar behavior was
previosuly reported for ohmic heating assisted extraction of orange juice
waste (Saberian, Hamidi-Esfahani, Ahmadi Gavlighi and Barzegar,
2017). This could be explained by the increasing mass transfer from
biological material to the solvent with increasing extraction time
(Colodel, Vriesmann, Teófilo, & de Oliveira Petkowicz, 2020).
From the Fig. 3A and Fig. 3B, it was concluded that the increasing
voltage gradient was increased the pectin yield from 10 V/cm to nearly
13.25 V/cm. However, further increase in voltage gradient resulted a
decrease in the pectin yield. The increasing trend from 10 to 13.25 V/cm
could be attributed to enhancing diffusion rate, caused by rupturing the
cell structure with increasing electrical field (Saberian, Hamidi-
Esfahani, Ahmadi Gavlighi and Barzegar, 2017). Similarly, de Oli­
veira, Giordani, Gurak, Cladera-Olivera, and Marczak (2015), reported
that the increasing electrical field strength caused an increase in the
pectin yield. However, increasing voltage gradient from 13.25 to 20 V/
cm caused a decrease in the pectin yield, possibly due to the disinte­
gration of extracted pectin with increasing heating rate and excessive
heating. A similar result was obtained by Ezzati, Ayaseh, Ghanbarzadeh,
and Heshmati (2020), who reported the pectin yield was decreased with
excessive heating conditions.
Interaction plots of the process factors for the pectin yield were
shown in Supplementary Fig. 1. Increased liquid to solid ratio was
increased the pectin yield at all extraction/ hydrodistillation time levels.
However, beyond a certain level pectin yield was decreased. This effect
may be seen more clearly in longer extraction times (45 and 60 min).
Similarly, at all voltage gradient levels, pectin yield was increased with
increasing liquid to solid ratio until to a certain level and then slightly
decreased. However, at 20 V/cm, decreasing trend of the pectin yield
was more dramatically. This may be related to the increase in the
amount of heat energy absorbed by the extracted pectin in the liquid
portion of the extraction medium due to presence of the less solid and
decreasing pectin concentration. The heating rate and time to reaching
to boiling point at 20 V/cm was far less than that of lower voltage
gradients. Thus, the higher heat exposure in the extraction OHAE/H
process especially higher voltage gradients and prolonged extraction
times may cause structural damage to the pectin and decreases the yield.
The increasing trends of pectin yield with increasing extraction/
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Innovative Food Science and Emerging Technologies 74 (2021) 102850
hydrodistillation times at all voltage gradient were similar, since the
interaction between extraction/hydrodistillation time*voltage gradient
was not significant. Also, the destructive effect of the increasing voltage
gradient was much more at higher liquid to solid ratios, possibly due to
excessive heating of the extracted pectin.
3.3. Effects of the OHAE/H variables on the essential oil yield
As presented in Table 2, linear effects of the all independent variables
were significant on the essential oil yield. The effects of the all inter­
action terms including liquid to solid ratio-extraction/hydrodistillation
time, liquid to solid ratio-voltage gradient and extraction/hydro­
distillation time-voltage gradient, were significant. The quadratic terms
have significant effect on essential oil yield except the quadratic term of
voltage gradient.
From the Table 2 and Fig. 2B.1, it was concluded that the most
effective linear variable on the essential oil yield was the extraction/
hydrodistillation time (F-value 136.80) followed by liquid to solid ratio
(F-value 104.25) and voltage gradient (F-value 21.84). The interactions
of liquid to solid ratio-voltage gradient and liquid to solid ratio-
extraction/hydrodistillation time was significant while the interaction
between the extraction/hydrodistillation time-voltage gradient was not
significant. The liqud to solid ratio and extraction/hydrodistillation time
showed a synergistic effect for the essential oil yield. However, all of the
significant interaction and quadratic terms with the voltage gradient
showed an unfavorable effect for essential oil yield (Fig. 2B.2).
As shown in the 3D response surface graphs and contour plots in the
Fig. 4, the essential oil yield gradually increased when the liquid to solid
ratio increased from 5:1 to 8:1. However, the liquid to solid ratio
exceeded 8:1 leading to the decrease in the essential oil yield. A proper
increase in the liquid to solid ratio could increase the essential oil yield
due to reducing mass transfer resistance and increasing desorption of
essential oil from the plant cells (Chen et al., 2020). The decreasing
trend of the essential oil yield with further increase in the liquid to solid
ratio may be explained by two mechanisms; overheating of plant ma­
terial and the increasing hydrolytic reactions due to the excessive water
content (Mollaei, Sedighi, Habibi, Hazrati, & Asgharian, 2019).
The increase in the extraction/hydrodistillation time has led to a
M.T. Tunç and H.İ. Odabaş Innovative Food Science and Emerging Technologies 74 (2021) 102850

corresponding increase in essential oil yield until approximately 50 min OHAE/H

(Fig. 4). However, the increase of extraction/hydrodistillation time after CHE/H
50 min caused a decrease in essential oil yield. This effect may possibly 100
due to the increasing hydrolytic reactions with the overheating of the
extraction medium and loss of the volatile compounds with increasing 98
extraction/hydrodistillation times (Liu, Ou, Xiang, & Gregersen, 2019).

Transmittance (%)
As seen in the Fig. 4, the increase in voltage gradient caused an in­ 96
crease in the essential oil yield. This result agree well with existing
94
studies on the hydrodistillation of clove (Tunç & Koca, 2019) and
oregano essential oils (Hashemi et al., 2017) by ohmic heating assisted 92
hydrodistillation. Due to the higher heating rate and shorter time to
reaching the boiling point at higher voltage gradients, the total accu­ 90
mulated essential oil was much more than lower voltage gradients
(Mohsen Gavahian, Farhoosh, Javidnia, Shahidi, & Farahnaky, 2015). In 88
addition, increasing voltage gradient may improve the electroporation
86
of the plant cell, thereby increase essential oil yield (Lebovka, Pra­
porscic, Ghnimi, & Vorobiev, 2005). 84
As could be seen in the Supplementary Fig. 2, the decreasing trends 4000 3500 3000 2500 2000 1500 1000
of the essential oil yield after a certain point of liquid to solid ratio and Wavenumber (1/cm)
voltage gradient was more dramatic at higher extraction/hydro­
distillation times and voltage gradient levels because of the increasing Fig. 5. FT-IR spectra of lemon waste pectin samples extracted by OHAE/H and
effects of aforementioned mechanisms (hydrolytic reactions and over­ CHE/H.
heating). The decreasing trend of the essential oil yield with increasing
extraction/hydrodistillation time can be seen more clearly especially in 3.6. Comparison of the OHAE/H and CHE/H
higher voltage gradients. The increase in the time of exposure to heat at
higher voltage gradients may have increased hydrolytic reactions. The 3.6.1. Physicochemical properties of pectin samples
increasing voltage gradient at relatively low liquid to solid ratios (5:1 Pectin yields of OHAE/H and CHE/H were 16.85 ± 0.28 and 15.47 ±
and 10:1) caused a gradual increase in the essential oil yield, while the 0.08, respectively. This result demonstrated that the pectin yield was
increasing voltage gradient at high liquid to solid ratio (15:1) caused a significantly increased by OHAE/H when compared CHE/H (p < 0.05).
decrease in the essential oil yield. Similarly, the increase in the voltage Compared to conventional method, ohmic heating assisted (or moderate
gradient in the longer extraction/hydrodistillation period caused a electric field assisted) extraction has been reported to produce higher
decrease in the essential oil yield, while the increase in the voltage pectin yield (de Oliveira et al., 2015; Saberian, Hamidi-Esfahani,
gradient in the relatively shorter extraction/hydrodistillation times Ahmadi Gavlighi and Barzegar, 2017).
increased the essential oil yield. Overheating of the plant material The galacturonic acid content of the pectin extracted by OHAE/H
during the OHAE/H could be reduced the yield specially at higher (69.38 ± 0.25) was found higher than CHE/H (65.72 ± 0.32) (p < 0.05).
voltage gradients and liquid to solid ratios (Mollaei et al., 2019). In Thermal profiles of the extraction medium during the OHAE/H and
addition, essential oils could be solubilized and chemically transformed CHE/H was shown in the Supplementary Fig. 3. The higher galacturonic
with increasing amount of extraction medium and prolonged heating acid content of the pectin extracted by OHAE/H could be explained by
due to the increasing liquid to solid ratio and voltage gradient the increasing hydrolysis of the pectin into galacturonic acid since the
(Milojević, Stojanović, Palić, Lazić, & Veljković, 2008). higher heating rate (thermal exposure) of the OHAE/H process (Oliveira
et al., 2016). Since their galacturonic acid contents was higher than
3.4. Multi-response optimization 65%, they could be classified as commercial pectin (May, 1990).
The degree of esterification of the pectin samples extracted by
Based on the results of the response surface analysis, a multi-
response optimization was done to achieve optimum OHAE/H condi­
tions which gave maximum pectin and essential oil yield. The desir­ OHAE/H
ability function method was used for optimization. The optimum OHAE/ CHE/H
H conditions were found to be: 8.7:1 liquid to solid ratio, 58.4 min 280
extraction/hydrodistillation time and 14.2 V/cm voltage gradient and
also, the maximum pectin and essential oil yields at these conditions
were 16.58 and 3.52 g/100 g lemon waste, respectively.
Heat flow (mW/g)

290

3.5. Verification experiments

300
The verification of the model equations for predicting the optimum
pectin and essential oil yield was experimentally tested using the opti­
mum conditions. The experimental values of pectin and essential oil 310
yields were found as 16.85 ± 0.28 and 3.61 ± 0.09 which were in
agreement with the predicted yields. Experimental values indicated that
the only 1.99% and 2.56% deviation between predicted and real values 320
of the pectin yield and essential oil yield, respectively. Thus the models
which explain the pectin yield and essential oil yield during OHAE/H Exo up 0 20 40 60 80 100 120 140 160 180 200 220 240 260 280
process were found suitable.
Temperature (°C)

Fig. 6. DSC thermograms of lemon waste pectin samples extracted by OHAE/H

and CHE/H.

7
M.T. Tunç and H.İ. Odabaş
Fig. 7. SEM scan of the pectin samples extracted by OHAE/H and CHE/H.
OHAE/H and CHE/H were 57.55 ± 0.28% and 59.45 ± 0.44%,
respectively. The extracted pectin samples by both of the extraction
methods could be classified as high methoxyl pectin since their esteri­
fication degree were greater than 50%. The lower esterification degree
of OHAE/H pectin could be explained by the higher de-esterification
rate of pectin because of the harsh temperature conditions of OHAE/H
(Wai, Alkarkhi, & Easa, 2010).
3.6.2. Ft-IR
FT-IR spectra presented in Fig. 5 showed that the extracted pectin
samples by OHAE/H and CHE/H had similar spectral profiles. The broad
bands between 3600 and 2400 cm− 1 could be related to the O-H
stretching due to inter- and intramolecular hydrogen bonding of the
galacturonic acid polymer (Gnanasambandam & Proctor, 2000). The
peaks at 3000 cm− 1 were indicative of methyl group stretching vibra­
tions from the methyl ester (Kalapathy & Proctor, 2001). The bands at
1730 and 1620 cm− 1 were related to esterified and free carbonyl groups,
respectively (W. Wang et al., 2015). The ratio of the peak area at the
1730 cm− 1 over the sum of the peak areas at the 1620 cm− 1 and 1730
8
Innovative Food Science and Emerging Technologies 74 (2021) 102850
cm− 1 correlated with the esterification degree of the pectin (Pappas
et al., 2004). Therefore, it could be concluded that the degree of ester­
ification of the pectin samples extracted by OHAE/H and CHE/H were
higher than 50% which in accordance with the results of the titrimetric
degree of esterification analysis.
3.6.3. Thermal properties of pectin samples
DSC thermograms of the pectin samples showed in the Fig. 6. As
shown in the Fig. 6, an endothermic peak, which was showed the
melting temperature, at 140 and 145 ◦ C were observed for OHAE/H and
CHE/H, respectively. Melting temperatures of the pectin samples
extracted in this study was in accordance with previous studies about
citrus pectin (W. Wang et al., 2016; X. Wang, Chen, & Lü, 2014). A slight
shift of endothermic peak toward higher temperature for CHE/H pectin
was probably due to its higher degree of esterification (Iijima, Naka­
mura, Hatakeyama, & Hatakeyama, 2000). The exothermic peak, cor­
responding to the degradation of pectin, observed for both pectin
samples at the same temperature (250 ◦ C) which were in accordance
with the degradation temperature for commercial citrus pectin recorded
M.T. Tunç and H.İ. Odabaş
Fig. 8. The flow behavior of the solutions of the pectins extracted by OHAE/H
and CHE/H.
Fig. 9. Frequency sweeps for the pectin solutions.
by Dranca and Oroian (2019).
3.6.4. Morphological properties of pectin samples
SEM analysis was performed to visualize the effects of the extraction
methods on the structures and morphology of the extracted pectin. Fig. 7
shows the SEM micrographs of the pectin samples. The distinct
morphological chactaristics among the pectin samples extracted by
OHAE/H and CHE/H could be seen in the Fig. 7. The structure of the
pectin extracted by CHE/H was more compact and smoother than the
pectin extracted by OHAE/H. However, the pectin extracted by OHAE/H
appears porous, rough and slightly ruptured form with spore like par­
ticles on the surface. Different morphological appearances of two pectin
samples extracted by OHAE/H and CHE/H possibly depending on the
differences of the extraction methods (Liew, Ngoh, Yusoff, & Teoh,
2016). Non-thermal effects of electric field (electroporation) might have
resulted in fragmentation on the pectin during the OHAE/H.
9
Innovative Food Science and Emerging Technologies 74 (2021) 102850
Fig. 10. Temperature sweeps for the pectin solutions.
3.6.5. Rheological properties of pectin samples
The flow behavior of the pectin solutions presented in Fig. 8. The
flow curves of pectin solutions were fitted by using the Power law model
successfully (R2 > 0.99). n values were found 1 and this was an evidence
of Newtonian behavior. Pectin solutions at low concentrations (up to
3%) exhibits Newtonian flow behavior. Pectin molecules are too far
away to interact with each other at diluted pectin solutions, so viscosity
of solution increases slightly (Chan, Choo, Young, & Loh, 2017). The
consistency coefficient (K) of CHE/H solutions higher than OHAE/E
solutions due to higher viscosity to compared OHAE/E solutions.
Apparent viscosity of CHE/H solutions were significantly (p < 0.05)
higher than OHAE/H solution. The viscosity of pectin solutions could be
linked with the degree of esterification, conformation, molecular
weight, source and charge density of pectin (Wan, Chen, Huang, Liu, &
Pan, 2019). Apparent viscosity is important criterion for the evaluation
of pectin stability and thickening (Wan et al., 2019). High viscosity
pectin solution is more suitable for use as a thickener. There are some
studies about pectin production by novel technologies, results indicated
that new technologies applied in pectin production are compared with
the conventional method, it has been reported by several researchers
that pectin solutions obtained by conventional method showed higher
viscosity (Khedmat et al., 2020; Yang, Chen, Yu, & Huang, 2020).
The storage modulus (G′ ), loss modulus (G′′ ) and tangent delta (tan
δ) values of pectin solutions at 0.1, 1 and 10 Hz were given at Fig. 9.
Storage and loss modulus were increased with raising frequency. At the
high frequency values, G′′ and tan delta values of CHE/H solutions are
significantly higher than OHAE/H solutions. At the low frequencies
extraction methods did not make any difference in G′ , G′′ and tan delta
values. According to Willemsen et al. (2017) the storage modulus (G′ )
express the stiffness of network, so it could be considered that there was
no significant difference between OHAE/H and CHE/H solutions in
terms of gel strong with a moderate stiffness. The ratio of G′′ / G′ refers to
tan delta and if the tan delta value is less than 1 this indicate that a
confirmation of the solid state of gels is obtained, if the tan delta value is
greater than 1 this indicate that the liquid state prevails and gels are
softer (Moreira et al., 2014). At the lower frequencies tan delta values,
higher than 1. These results showed that pectin solutions had a soft gel
structure at low frequencies, whereas it has a harder structure at high
frequency values.
When the effect of temperature on elasticity properties were exam­
ined, G′′ values of CHE/H solution was higher than OHAE/H solutions
(Fig. 10). Nevertheless, at the higher temperature, there was no signif­
icant difference between two pectin solutions in terms of loss modulus.
M.T. Tunç and H.İ. Odabaş Innovative Food Science and Emerging Technologies 74 (2021) 102850

Table 3
Chemical compounds of lemon essential oils.
Compounds CHE/H OHAE/H
a
1 1,4-Cyclohexadiene,1-methyl 0.26 ± 0.36 0.00 ± 0.00b
2 α-phellandrene 0.34 ± 0.03a 0.33 ± 0.01a
3 α-Pinene 1.16 ± 0.12a 1.18 ± 0.01a
4 Camphene 0.14 ± 0.01a 0.08 ± 0.00b
5 Sabinene 0.24 ± 0.02a 0.16 ± 0.14a
6 β-Pinene 2.50 ± 0.29a 3.33 ± 0.20a
7 Myrcene 1.69 ± 0.01a 1.67 ± 0.01a
8 α-terpinene 0.70 ± 0.08a 0.49 ± 0.00b
9 Limonene 70.02 ± 0.60b 71.76 ± 0.52a
10 γ-Terpinene 9.79 ± 0.17a 9.94 ± 0.18a
11 Terpinolene 1.45 ± 0.13a 0.97 ± 0.00b
12 Linalol 0.40 ± 0.05a 0.48 ± 0.01a
13 Nonanal 0.03 ± 0.00a 0.03 ± 0.00a
14 Fenchyl alcohol 0.24 ± 0.22a 0.07 ± 0.00a
15 Cyclohexanol,1-methyl-4-(1- 0.48 ± 0.15a 0.20 ± 0.01a Fig. 11. Total extracted pectin and essential oil per 100 kJ consumed energy.
methylethenyl)
16 α-Terpineol 4.62 ± 0.98a 2.42 ± 0.11a
lemon essential oil. OHAE/H was significantly (p < 0.05) enhanced the
17 Geraniol 0.08 ± 0.01b 0.15 ± 0.01a
18 Citral 0.38 ± 0.07b 0.71 ± 0.04a limonene peak area of lemon essential oil when compared to CHE/H. M.
19 Citronellyl butyrate 0.12 ± 0.01a 0.12 ± 0.00a Gavahian et al. (2018) were extracted essential oil from Taiwanese
20 Geranyl butyrate 0.81 ± 0.05a 0.89 ± 0.02a citronella T grass and they reported that ohmic heating assisted hydro­
21 Nerol cis geraniol 0.86 ± 0.06a 0.99 ± 0.02a distillation method enhanced the area of D-limonene from 1.8% to 3.3%.
22 β-Caryophyllene 0.21 ± 0.03a 0.25 ± 0.01a
23 Bicyclo [3,1,1]hept-2-ene,2,6-dimethyl-6 0.48 ± 0.07a 0.57 ± 0.02a
Differences between chemical compounds could be due to particularly
24 Valencene 0.27 ± 0.03a 0.30 ± 0.01a isomerization, oxidation dehydrogenation, thermal rearrangements,
25 Bisabolene 0.74 ± 0.10a 0.81 ± 0.02a polymerization, thermal and hydrolysis reactions (Tunç & Koca, 2019).
Total 98.21 ± 0.16a 98.37 ± 0.15a
3.6.7. Energy consumption
The total energy consumptions for OHAE/H (at optimum conditions)
Pectin solutions showed an increase of the storage modulus with
and CHE/H were 983.76 ± 13.90 and 1042.22 ± 1.80 kJ, respectively.
increasing temperature. This could be due to changes in macromolecule
Energy consumption of OHAE/H was significantly lower than CHE/H
conformation during heating (Moreira et al., 2014). Gel point which is
method (p < 0.05). The lower energy consumption of OHAE/H could be
defined as in accordance with the temperature at which G′ = G′′ (Con­
related with internal and uniform heat generation (Kanjanapongkul,
stenla, Ponce, & Lozano, 2002). G′ and G′′ values were cross over at
2017). Total extracted pectin and essential oil per 100 kJ energy was
critical temperature 48.5 ◦ C and 51.2 ◦ C for OHAE/H and CHE/H so­
calculated for the comparison of the efficiencies of the OHAE/H and
lutions respectively. Hydrogen bonds in the structure of galacturonic
CHE/H (Fig. 11). As shown in the Fig. 11 total extracted pectin and
acid units are the basic structures to provide gel structure, but they are
essential oil per 100 kJ consumed energy for OHAE/H were 15.54% and
insufficient to overcome the entropic barrier formed for gelation.
65.22% higher than CHE/H method, respectively.
Studies reported that hydrogen bonds and hydrophobic interactions
were eased at an intermediate temperature range to provide higher
elasticity (Chan et al., 2017). 4. Conclusion

3.6.6. Essential oil yield and composition
The essential oil yields were 3.69 ± 0.09 and 2.44 ± 0.19 for OHAE/
H and CHE/H, respectively. The essential oil yield of the OHAE/H
method was significantly higher than the CHE/H method (p < 0.05). The
higher essential oil yield could be attributed to lower time of the
reaching the boiling point during OHAE/H and the electroporation ef­
fect of the electrical field used in the OHAE/H process. Table 3 reports
the results obtained from GC–MS analysis of lemon essential oils
extracted by CHE/H and OHAE/H methods. Data was expressed as peak
areas of components. Aroma composition of lemon essential oils
extracted with different methods have similar components. A total of 25
and 24 chemical components which expressed more than 98% of total
lemon essential oil, were identified in the lemon waste essential oil
extracted by CHE/H and OHAE/H methods, respectively. Limonene
(70.02–71.76%) and γ-terpinene (9.79–9.94%) were the major compo­
nents. α-Pinene (1.16–1.18%), β-Pinene (2.50–3.33%), Myrcene
(1.69–1.67), Terpinolene (1.45–0.97%) and α-terpineol (4.62–2.42%)
were in intermediate concentration. Other compounds were identified
as minor compounds. Researchers reported that limonene was the main
component in lemon essential oil, its peak areas varied according to
variety of lemon, environmental conditions, geographical distribution
and extraction method (Martínez-Abad et al., 2020; Paw, Begum, Gogoi,
Pandey, & Lal, 2020; Pellizzeri, Costa, Grasso, & Dugo, 2020). Ribeiro-
Santos et al. (2018) was reported limonene (62.12%), β-pinene
(14.34%) and γ-terpinene (8.88%) were found as a main component in
In the present study, ohmic heating assisted extraction/hydro­
distillation method to simultaneously extraction of the pectin and
essential oil from lemon waste was investigated for the first time.
Response surface methodology was successfully applied for the opti­
mization of the OHAE/H conditions and the estimation of the effects of
the process factors on pectin and essential oil yields. Optimum OHAE/H
conditions were as follows: 8.7:1 liquid to solid ratio, 58.4 min extrac­
tion/hydrodistillation time and 14.2 V/cm voltage gradient. The most
effective process factor on the pectin and essential oil yields was liquid
to solid ratio and extraction/hydrodistillation time, respectively. The
optimal pectin and essential oil yields was 16.58 and 3.62 g/100 g lemon
waste (dry weight), respectively. This study provided a novel, efficient
and economic method for pectin and essential oil extraction from lemon
waste and the resulting pectin and essential oil could be employed as
food ingredients. Application of OHAE/H dramatically increased pectin
and essential oil yields when compared conventional heating method.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.

10
M.T. Tunç and H.İ. Odabaş
org/10.1016/j.ifset.2021.102850.
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