LWT - Food Science and Technology 153 (2022) 112549

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LWT
journal homepage: www.elsevier.com/locate/lwt

Cinnamomum camphora fruit peel as a source of essential oil extracted using

the solvent-free microwave-assisted method compared with
conventional hydrodistillation
Zaizhi Liu a, *, Hualan Li a, Zheng Zhu a, Dai Huang a, Yanlong Qi b, Chunhui Ma c,
Zhengrong Zou a, Hiyan Ni a, **
a
College of Life Sciences, Jiangxi Normal University, Nanchang 330022, China
b
Key Laboratory of High-Performance Synthetic Rubber and Its Composite Materials, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Renmin
Road, Changchun 130022, China
c
Key Laboratory of Bio-based Material Science & Technology, Northeast Forestry University, Harbin 150040, China

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

Keywords: In the present study, essential oil from Cinnamomum camphora fruit peel was first separated and characterized by
Solvent-free microwave-assisted extraction GC-MS. Solvent-free microwave-assisted extraction (SFME) was performed to isolate the essential oil, and the
Essential oil extraction procedure was optimized using a Box–Behnken design. The optimum SFME conditions yielded 80.35
Cinnamomum camphora fruit peel
± 1.88 mg/g of essential oil with 76% moisture content, using a microwave irradiation power of 420 W and an
Kinetic study
Chemical composition
irradiation time of 22 min. No obvious difference was observed between physical constants of essential oil
extracted by SFME and hydrodistillation (HD). Scanning electron microscopy micrographs demonstrated more
disruption of C. camphora fruit peel cells treated with SFME than by conventional HD. SFME was proposed as an
energy-saving, high-efficiency, and environmentally friendly method, as evidenced by its higher yield and
volumetric mass transfer coefficient, larger proportions of oxygen compounds, lower consumption of electricity,
and lower amounts of CO2 release and water waste compared to conventional HD. The results show that a once-
discarded part of C. camphora can be utilized as a source for the production of essential oil.

1. Introduction
Essential oil, also known as volatile oil, is a complex mixture of low
molecular weight components separated from aromatic plants, charac­
terized by a strong odour (Cassel, Vargas, Martinez, Lorenzo, & Della­
cassa, 2009; Meziane, Maizi, Abatzoglou, & Benyoussef, 2020). Essential
oils have been used in Ayurveda and traditional Chinese medicine to
treat many diseases (Bakkali, Averbeck, Averbeck, & Idaomar, 2008).
Essential oils possess many remedial advantages, including antioxidant
(Meullemiestre, Kamal, Maache-Rezzoug, Chemat, & Rezzoug, 2014),
antibacterial (He et al., 2020), antifungal (Moazeni et al., 2021),
anti-inflammatory (Menichini et al., 2009), antitumor and antiviral ac­
tivities (Raut & Karuppayil, 2014), which make them promising in drug
discovery and drug development (Raut & Karuppayil, 2014) and for use
in food enrichments, food fortifiers, antioxidants, and food flavoring and
preserving agents in the food industry (Bajalan, Rouzbahani, Pirbalouti,
& Maggi, 2018; Ghasemi Pirbalouti, Craker, & Alavi-Samani, 2018;
Giacometti et al., 2018).
Essential oil is generally separated using physical methods, such as
solvent extraction, traditional hydrodistillation (HD), and steam distil­
lation (Chouhan, Tandey, Sen, Mehta, & Mandal, 2019). However, these
approaches have several shortcomings, including time and energy con­
sumption and low extraction yield (Giacometti et al., 2018). An
economical and efficient technology resulting in the highest extraction
yield of the target compounds in the shortest treatment time using the
lowest amount of energy will inevitably be favored. Microwave irradi­
ation is widely applied in the process of extracting plant natural com­
pounds with the merits of saving time and energy and improving yield
compared to traditional methods (Elik, Yanık, & Göğüş, 2020; Liu et al.,
2021; Lucchesi, Chemat, & Smadja, 2004a; Macedo et al., 2021; Nabil
et al., 2009; Vian, Fernandez, Visioni, & Chemat, 2008; Yanık, 2017).
Solvent-free microwave extraction (SFME) was first proposed by

* Corresponding author.
** Corresponding author.
E-mail addresses: zaizhiliu@hotmail.com (Z. Liu), nihaiyan16@163.com (H. Ni).

https://doi.org/10.1016/j.lwt.2021.112549
Received 9 July 2021; Received in revised form 26 September 2021; Accepted 27 September 2021
Available online 3 October 2021
0023-6438/© 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Z. Liu et al. LWT 153 (2022) 112549

Lucchesi et al. (2004a) and combines microwave irradiation with

distillation. It is generally carried out at normal pressure. In the SFME
procedure, fresh or previously moistened dried plant materials were
directly placed in a microwave extraction apparatus with no additional
solvent, which facilitated subsequent processing (Ma, Yang, Zu, & Liu,
2012; Sui et al., 2012). When the microwave radiation heated the in situ
water contained in the plant materials, the inner pressure of the cells
increased dramatically, resulting in rupture of the cell wall and release
of the essential oil. SFME has already been employed to separate plant
essential oils (Benmoussa, Farhat, Romdhane, & Bouajila, 2019; Bouk­
roufa, Boutekedjiret, Petigny, Rakotomanomana, & Chemat, 2015;
Michel, Destandau, & Elfakir, 2011) due to its advantages of solvent
elimination, high extraction efficiency, high quality of the obtained
essential oils, and safe and green impact on the environment compared
to traditional hydrodistillation (HD) (Bayramoglu, Sahin, & Sumnu,
2008; Liu, Deng, Li, & Zou, 2018; Lucchesi et al., 2004a). Herein, SFME
is of great interest to isolate essential oil from Cinnamomum camphora
fruit peel.
C. camphora, a member of the Lauraceae family, is an evergreen tree
species primarily distributed in subtropical or tropical zones, such as
southern China and Korea, Japan, Vietnam, and India (Zhang et al.,
2020). C. camphora fruit is important in China. More than 1 million tons
of seeds are harvested per year. They have been widely consumed in
parts of China south of the Yangtze River since the 1960s (Yan et al.,
2020; Zhang et al., 2020). Therefore, a large amount of C. camphora fruit
peel is produced as byproducts every year, which is currently discarded,
resulting in environmental pollution and wasted plant resources. The
whole C. camphora plant contains valuable essential oil (Guo et al.,
2016; Jiang et al., 2016; Wang et al., 2019) that is used in many in­
dustries, including the spice, food, and pharmaceutical industries (Lee
et al., 2006; Sokolova et al., 2015; Zarubaev et al., 2015). Thus far, much
attention has been given to the investigation of C. camphora leaf
essential oil. To date, no report has examined the extraction of essential
oil from C. camphora fruit peel.
This study aimed to extract essential oil from C. camphora fruit peel
using SFME. The extraction process was optimized by a Box–Behnken
design (BBD) of response surface method (RSM). Traditional HD was
performed for comparison. GC-MS was carried out to characterize the
chemical components of essential oil extracted by SFME and traditional Fig. 1. Schematic diagram of the SFME apparatus.
HD. A kinetic study was performed to calculate the volumetric mass
transfer coefficients of the two extraction procedures. The environ­ experimental trials, the microwave oven was set to different irradiation
mental impacts of SFME and HD were investigated in terms of electricity powers and times as required. Specifically, the nominal microwave
consumption and amount of CO2 released and wastewater produced. power was used to express the microwave power. When the extraction
system temperature reached the boiling point of water, the vapor from
2. Materials and methods the in situ water contained in C. camphora fruit peel evaporated upward
out of the round-bottom flask, carrying essential oil, passed through a
2.1. Materials condenser located on the top of the extraction vessel, quickly condensed
into liquid, and then collected in an oil–water separator while the mixed
Mature C. camphora fruit was picked from trees on the Jiangxi vapor met the reflux condenser. The oil and water naturally separated
Normal University campus (Nanchang, China) in December 2020 and into two layers, with the essential oil in the upper layer. After the
authenticated by Professor Yisheng Tu (Jiang Xi Normal University, extraction process finished, the water was released, and the essential oil
Nanchang, China). The fresh fruit was immediately separated into peel was collected in a centrifuge tube. The obtained essential oil was stored
and seeds, and the C. camphora fruit peel was stored in a refrigerator at at 4 ◦ C until analysis. The essential oil yield was calculated by Eq. (1):
4 ◦ C for the following experiments.
Yield (mg / g) = m / M (1)
2.2. SFME procedure for extraction of essential oil from C. camphora
fruit peel where m and M are the mass of the obtained essential oil (mg) and the
dry weight of C. camphora fruit peel for each extraction (g), respectively.
A schematic diagram of the SFME apparatus is illustrated in Fig. 1.
An SFME apparatus was employed to isolate essential oil from 2.3. Experimental design
C. camphora fruit peel, as described in our previous study (Liu et al.,
2018). C. camphora fruit peel was soaked in distilled water to reach the To investigate the SFME procedure and maximize the essential oil
moisture content in the experimental design, as described in a previous yield, BBD was applied to optimize the extraction conditions of three
study (Benmoussa et al., 2018). Then, 200 g of fresh C. camphora fruit parameters: moisture content (A), microwave irradiation power (B) and
peel was added to a 1 L round-bottom flask and then transferred to a microwave irradiation time (C). To determine the interaction effects of
microwave oven for essential oil extraction. Throughout the the three parameters, 12 free combinations accompanied by five

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Z. Liu et al. LWT 153 (2022) 112549

Table 1 essential oil was performed by a Thermo Trace-1300 ISQ-mass chro­

Coded and real levels of screened parameters and observed responses. matograph (Thermo Fisher Scientific Inc., Waltham, MA, USA) equipped
Runa A B C Yield (mg/g) with an HP-5 MS capillary column (30 m × 0.25 mm, 0.25 mm i.d., film
thickness 0.2 μm). The temperatures for the injector and detector were
Predicted Actual
preset at 230 ◦ C and 280 ◦ C, respectively. The temperature rise program
1 75 385 20 70.54 68.92 began at 60 ◦ C for 5 min, increased to 120 ◦ C at 10 ◦ C/min for 5 min,
2 70 385 25 69.52 70.54
3 70 540 20 71.36 69.75
increased to 200 ◦ C at 10 ◦ C/min for 5 ◦ C/min, and finally increased to
4 75 540 25 63.57 64.16 280 ◦ C at 10 ◦ C/min, where it was maintained for 15 min. The carrier
5 75 385 20 70.54 71.35 gas was helium at an initial flow of 1 mL/min. For analysis, 10 μL of
6 75 540 15 65.91 65.25 essential oil diluted in methanol (1:500, v/v) was injected in split mode
7 80 385 25 77.55 75.28
(1:2). MS was performed in EI mode at 70 eV with a scan range of
8 70 385 15 68.6 70.87
9 75 385 20 70.54 72.05 50–500 amu. Identification of the essential oil components was based on
10 75 230 15 41.9 41.31 the NIST mass spectral library by comparing the mass spectral pattern
11 70 230 20 47.26 45.58 and retention indices. The percentage of chemical composition was
12 80 230 20 58.64 60.25 quantified by normalization to the peak areas.
13 75 385 20 70.54 68.85
14 80 385 15 63.47 62.45
15 75 385 20 70.54 71.51
2.7. Physical analysis
16 75 230 25 59.22 59.88
17 80 540 20 62.89 64.57
a
The physical properties of the C. camphora fruit peel essential oil
A: Moisture content, %; B: Microwave power, W; C: Microwave time, min.
obtained through SFME and HD were analyzed. The physical constants
defining essential oil, including density and optical rotation, were
replicates (center point) were performed on the basis of the three levels determined at 20 ◦ C (Bousbia et al., 2009).
(− 1, 0, and +1), as shown in Table 1. The entire SFME process for
obtaining C. camphora fruit peel essential oil was digitally described by 2.8. Scanning electron microscopy (SEM) analysis
the quadratic polynomial equation model in Eq. (2): The morphologies of C. camphora fruit peel (before and after
∑
3 ∑
3 2 ∑
∑ 3 extraction by HD and SFME) were recorded on an S–3400N scanning
Y = β0 + β i Xi + βii Xi 2 + βij Xi Xj (2) electron microscope (HITACHI, Tokyo, Japan).
i=1 i=1 i=1 i=1

where Y expresses the predicted yield (mg/g), Xi and Xj denote the coded
variables, β0 represents the constant coefficient, and βi, βii and βij signify
the coefficients of the linearizing, second-order and interactive terms,
respectively.
2.4. Comparison of SFME with HD
Traditional HD was operated in a Clevenger-type apparatus con­
nected with an essential oil extractor. C. camphora fruit peel (200 g) was
placed in the sample flask and then heated for 4 h by a heating jacket at
1 kW h. The moisture content of the fruit peel was based on the obtained
optimal conditions, and the other procedures were the same as SFME.
2.5. Kinetic model
2.9. Environmental impact of SFME and HD
The electricity consumption, amount of CO2 released, and water
consumption were calculated to determine the environmental impact of
the SFME and HD extraction processes.
The electricity consumption (EC) of SFME and HD was calculated as
the electricity power by time using Eq. (4):
EC = P × t (4)
where EC represents electrical consumption (kW h), and P and t repre­
sent the electricity power (kW) and time (h), respectively.
According to Vian et al. (2008), 800 g of CO2 will be discharged into
the ambient air to produce 1 kW h by combusting coal or fuel. Hence, the
CO2 release amount (RAco2) can be calculated by Eq. (5):

Handayani, Sutrisno, Indraswati, and Ismadji (2008) proposed that RAco2 = A × 800 (5)
the dominant mechanism restraining the extraction rate is mass transfer
of target substances from the solid plant materials to the solvent, which where RAco2 represents the amount of CO2 released (kg), and A repre­
describes the mechanism controlling the extraction of C. camphora fruit sents electricity consumption (kW h).
peel essential oil. Based on Fick’s law, a first-order kinetic model Eq. (6) was used to calculate the amount of wastewater generated
employed to fit the experimental data is presented in Eq. (3): during the two extraction processes (Farhat et al., 2017):

Y = Ye [1 − exp( − kL ⋅ a ⋅ t)] (3)

Wastewater ​ amount ​ = ​ Volume ​ of ​ water ​ consumption ​ / ​ Total ​ mass ​ of ​ essential ​ oil (6)

where Y and Ye (mg/g) signify the C. camphora fruit peel essential oil
yields at any time and at equilibrium time, respectively, kL⋅α signifies the
volumetric mass transfer coefficient, and time is expressed by t (min).
2.6. Chemical composition of essential oil
Quantification of volatile compounds in C. camphora fruit peel
2.10. Statistical analysis
Design Expert 8.0 software (Stat Ease Inc., Minneapolis, MN, USA)
was employed for process design optimization, regression analysis and
depiction of the response surface plots. Essential oil yields were
conveyed as the average value ± standard deviation of three indepen­
dent operations and statistically evaluated by analysis of variance
(ANOVA) using OriginPro 2018 software (OriginLab Corporation,

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Z. Liu et al. LWT 153 (2022) 112549

Northampton, MA, USA).
3. Results and discussion
3.1. Single-factor experiments
3.1.1. Influence of moisture content
In the SFME process, plant essential oil is entrained by the inner
water through azeotropic distillation (Lucchesi, Chemat, & Smadja,
2004b). To evaluate the influence of moisture content on the SFME
process, experiments were carried out with moisture content ranging
from 60% to 85% at a microwave irradiation time of 20 min and irra­
diation power of 385 W. As shown in Fig. 2a, the yield of C. camphora
fruit peel essential oil improved with the initial increase of moisture
content, while a decrease was observed when the moisture content
exceeded 75%. This phenomenon was attributed to the fact that a low
moisture content could result in a slow speed of evaporation and further
brought about a lower yield of essential oil, whereas a high moisture
content could cause some compounds to dissolve in the water and hy­
drolyze (Qi et al., 2014). Consequently, moisture contents ranging from
70% to 80% were determined to be the appropriate levels for the
extraction process.

3.1.2. Influence of microwave irradiation power

The variable of microwave irradiation power was studied to find the
suitable level in the SFME procedure for further optimization. Fig. 2b
shows that microwave irradiation power demonstrated a quadratic ef­
fect on C. camphora fruit peel essential oil yield, which exhibited a strong
uptrend as the microwave irradiation power ranged from 120 W to 385
W and then a downtrend when the microwave irradiation power rose
from 380 W to 700 W. When the plant materials suffered from thermal
stresses and high pressure triggered by microwave irradiation, the inner
plant cells were more easily destroyed and thus released essential oil;
however, a high level of microwave irradiation power may cause
degradation of the volatile compounds (Ma et al., 2011; Patil & Aka­
manchi, 2017). Hence, the suitable range of microwave irradiation
power was within 385 W–540 W.

3.1.3. Influence of microwave irradiation time

The experiments were operated under various microwave irradiation
times ranging from 5 min to 30 min at a fixed moisture content of 75%
and a microwave irradiation power of 385 W, and the results are pre­
sented in Fig. 2c. The C. camphora fruit peel essential oil yield increased
observably with increasing microwave irradiation time from 5 min to 20
min, and then the yield increased insignificantly with microwave irra­
diation time over 20 min. In view of energy consumption, 20 min–25
min was determined to be the appropriate range of microwave irradia­
tion time for further optimization.

3.2. Optimization of SFME

3.2.1. Fitting the response surface model

Fig. 2. Influences of water moisture (a), microwave irradiation power (b), and
microwave irradiation time (c) on the yield of essential oil from C. camphora
fruit peel.
The mutual interactions between the C. camphora fruit peel essential
oil yield and the three parameters of moisture content, microwave
irradiation power and time were further investigated by the quadratic
polynomial equation, and the running results are displayed in Table 1.
The variance analysis (ANOVA) results are presented in Table 2. The
significance of each coefficient was evaluated by the F value and P-
value, and a high F value and low P-value denote a significant influence
of each term (Pongsumpun, Iwamoto, & Siripatrawan, 2020). The
P-value of 0.1272 for the lack-of-fit test meant it was insignificant for
essential oil yield and indicated that the developed model fit well with
the experimental data and could accurately predict the variation (Bel­
hachat, Mekimene, Belhachat, Ferradji, & Aid, 2018). A high R2 value
(0.9747) indicated that the developed model was very efficient for
fitting the obtained data under the operating conditions, and the
adjusted R2 value (0.9422) implied perfect accordance between the
predicted and actual values of the developed model for the essential oil
yield (Table 2). This illustrated that the developed model is capable of
studying the linear, interactive, and quadratic influences of moisture
content, microwave irradiation power and time on the C. camphora fruit
peel essential oil yield and optimizing the SFME process with desirable
responses.
According to Table 2, the linear effect of microwave irradiation
power and the quadratic effect of microwave irradiation power were
extremely significant (P-value < 0.001), the linear effect of microwave
irradiation time and the interaction effect of moisture content versus

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Table 2
Analysis of variance (ANOVA) for the experimental resultsa.
Source Sum of squares Degree of freedom Mean square F value P value
b
Model 1316.07 9 146.23 29.98 <0.0001***
A 4.22 1 4.22 0.86 0.3833
B 402.00 1 402.00 82.41 <0.0001***
C 112.35 1 112.35 23.03 0.0020**
AB 98.51 1 98.51 20.19 0.0028**
AC 43.30 1 43.30 8.88 0.0205*
BC 96.63 1 96.63 19.81 0.0030**
A2 2.82 1 2.82 0.58 0.4720
2
B 539.24 1 539.24 110.54 <0.0001***
C2 10.37 1 10.37 2.13 0.1882
Residual 34.15 7 4.88
Lack of fit 24.79 3 8.26 3.53 0.1272
Pure error 9.36 4 2.34
Cor totalc 1350.22 16
Credibility analysis of the regression equations
Std. Dev.d Mean C.V. e % Press R2 Adjust R2 Predicted R2 Adequacy precision
2.21 64.86 3.41 411.27 0.9747 0.9422 0.6954 21.045

*p < 0.05, significant; **p < 0.01, highly significant; ***p < 0.001, extremely significant.
a
The results were obtained with the Design Expert 8.0 software.
b
A: Moisture content, %; B: Microwave power, W; C: Microwave time, min.
c
Totals of all information corrected for the mean.
d
Standard deviation.
e
Coefficient of variation.

microwave irradiation power were highly significant, as evidenced by
their P-values (P < 0.01), and the interaction effect of moisture content
versus microwave irradiation time (P < 0.05) showed a significant effect
on C. camphora fruit peel essential oil yield. The linear effect of moisture
content and the interaction effect of moisture content versus microwave
irradiation time were significant. The linear effect of moisture content
and the quadratic effects of moisture content and microwave irradiation
time did not influence the yield of C. camphora fruit peel essential oil.
The significant items were thus included in the quadratic polynomial
equation (Eq. (7)) to clarify the C. camphora fruit peel essential oil yield
as follows:
as they were totally within the allowable range, that is, ± 3.0.
3.2.3. Response surface analysis
Three-dimensional and contour surface plots were applied to visually
magnify the mutual effects of the two variables, as shown in Fig. 4. The
effects of moisture content and microwave irradiation power on
C. camphora fruit peel essential oil extraction (Fig. 4a) indicated that the
maximum yield (76.78 mg/g) was obtained at a moisture content of 75%
and a microwave power of 439 W. Further increases in moisture content
and microwave power tended to decrease the essential oil yield. The
reason may be that sharp heating by a relatively high power could cause

Yield = 75.34 ​ + ​ 8.59B ​ + ​ 5.96C ​ − ​ 2.21AB ​ − ​ 0.89AC ​ − ​ 3.17BC ​ − ​ 5.74A2 ​ − ​ 12.80B2 ​ − ​ 3.13C2 ​ (7)

3.2.2. Investigating model adequacy
The model adequacy was tested by depicting the three diagnostic
plots. A normal probability plot can clearly denote whether the residuals
follow the normal distribution, and the points should lie on or near the
straight line rather than following any sequence or trend (Abdulrahman,
2021). As shown in Fig. 3a, all the points surround the straight line, and
the residuals for the responses of essential oil yield conform to normal
distribution, which reveal that the developed model presents a good
approximation of the actual essential oil yield. The residuals versus run
numbers (Fig. 3b) were constructed to investigate the response and its
satisfactory fit (Sodeifian, Sajadian, & Ardestani, 2017). The diagnostic
plot showed that all the data were reliable, as they were totally within
the allowable range, that is, ± 3.0. The plot of predicted versus actual
values is depicted in Fig. 3c to estimate the model compatibility
(Sodeifian et al., 2017). The predicted values and the actual values
exerted a high degree of fitting, as all the data were located on a straight
line. Meanwhile, the results also showed that the model possessed a
good optimization effect on the extraction conditions of C. camphora
fruit peel essential oil. The residuals versus run numbers (Fig. 3b) were
constructed to investigate the response and its satisfactory fit (Sodeifian
et al., 2017). The diagnostic plot showed that all the data were reliable,
fast destruction of the plant cells (Kapadiya, Parikh, & Desai, 2018),
while an extremely high microwave irradiation power could trigger the
decomposition of the inner compounds (Boukroufa et al., 2015; Patil &
Akamanchi, 2017) and thus affect essential oil yield. The interactive
effects of moisture content and microwave irradiation time on
C. camphora fruit peel essential oil extraction with microwave irradia­
tion power at a central level are displayed in Fig. 4b. The essential oil
yield showed a strong increase with increasing moisture content and
microwave irradiation time, and a slight decrease was seen with
increasing moisture content and microwave irradiation time beyond
75% and 23 min, respectively. This is likely because some volatile
components in the essential oil disintegrated under a higher moisture
content; however, a lower moisture content may result in a reduction of
the evaporation rate of in situ water (Cui et al., 2017). The interaction
effect of microwave irradiation power and time showed a quadratic ef­
fect on essential oil yield with moisture content at a central level of 75%,
as shown in Fig. 4c. The essential oil yield increased with the initial
increase in microwave irradiation power and time (below 415 W and 23
min), and further increasing these two variables resulted in a decrease.
Lower microwave irradiation power and shorter microwave irradiation
time may lead to insufficient recovery of essential oil, while higher
microwave power may cause the pyrolysis or decomposition of essential
oil (Benmoussa, al., 2018; Chouhan et al., 2019).

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Fig. 4. The three-dimensional and contour surface plots from BBD. (a) The
effects of moisture content and microwave irradiation power on C. camphora
fruit peel essential oil extraction; (b) the interactive effects of moisture content
and microwave irradiation time on C. camphora fruit peel essential oil extrac­
Fig. 3. Diagnostic plots for model adequacy checking. Normal probability plot
tion; and (c) the interaction effect of microwave irradiation power and time on
(a), residuals versus run number (b), and predicted versus actual (c).
C. camphora fruit peel essential oil extraction.

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Z. Liu et al.
Fig. 5. Mass transfer kinetics curves and temperature profile as a function of time of SFME and HD for extraction of C. camphora fruit peel essential oil. Insert:
experimental data, fitting of mass transfer kinetic model, and the parameters of Ye and kL⋅α.
3.2.4. Verification tests of the models
Process optimization is interactive and examines the statistical
agreement between the parameters and the corresponding response
(Agu, Menkiti, Kadurumba, & Menkiti, 2015). In this experiment, a BBD
of RSM was employed to model the interactions between the SFME
conditions (moisture content, microwave irradiation power and time)
and the response (essential oil yield). Based on the BBD results, the
optimal conditions to achieve the maximum essential oil yield (78.30
mg/g) from C. camphora fruit peel were 76% moisture content, 421 W
microwave irradiation power, and 22 min microwave irradiation time.
Experiments were performed under the obtained conditions with slight
modification (420 W of microwave irradiation power) to verify the
proposed solution by determining the actual yield. The actual essential
oil yield obtained was 80.35 ± 1.88 mg/g, which agrees with the
theoretical yield. This result indicated that the employed model was
adequate and satisfactory for optimizing the SFME process.
3.3. Kinetic studies of SFME and HD
Fig. 5 shows the extraction kinetic curves of SFME and HD for
obtaining essential oil from C. camphora fruit peel. The kL⋅α value of the
parameter of SFME was much higher than that of HD. Diffusion is
affected by the extraction system temperature (Liu et al., 2016); the
SFME method can quickly increase the temperature to 100 ◦ C under
microwave irradiation, while the HD method took 30 min to reach the
boiling point. Increasing the diffusion coefficient enhances the mass
transfer rate of target compounds from plant materials inside to outside.
Therefore, the essential oil yield by SFME (22 min and 420 W for 80.35
± 1.88 mg/g) showed an apparent improvement compared to that of HD
(240 min and 1000 W for 75.19 ± 1.45 mg/g). A similar outcome was
observed using the SFME procedure to obtain Amomum tsao-ko essential
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LWT 153 (2022) 112549
oil (Cui et al., 2017) and Tunisian cumin seed essential oil (Benmoussa
et al., 2018). The main principle behind this phenomenon is that the in
situ water molecules inside the plant material constantly collide and rub
under the irradiation of electromagnetic waves in the SFME process,
which rapidly improves the internal temperature and pressure of plant
cells and thereby triggers cell disruption.
Périno-Issartier, Ginies, Cravotto, and Chemat (2013) reported that
the essential oil yield obtained by 15 min of the microwave hydro­
diffusion and gravity method was significantly higher than that acquired
from 4 h of steam distillation. Farhat et al. (2017) employed four
extraction methods (microwave-assisted HD, SFME, steam distillation
and HD) to extract rosemary oil and found that microwave irradiation
provided faster extraction in a shorter time in the SFME and
microwave-assisted HD trials. Vian et al. (2008) reported that the
extraction process involving microwave energy could reduce the
extraction time from 3 h of HD to 15 min of the microwave hydro­
diffusion and gravity method without changing the essential oil
composition. These results all illustrated that the introduction of mi­
crowave irradiation in SFME is a promising alternative to HD for the
efficient separation of plant essential oil with the merits of improving
yields and shortening the extraction time.
3.4. Chemical composition of essential oil
The total ion chromatograms of the C. camphora fruit peel essential
oil obtained by SFME and HD are given in Fig. 6. The chemical
composition of the essential oil is summarized in Table 3. Thirty-five
compounds with a total proportion of 97.19% were characterized in
C. camphora fruit peel essential oil obtained by SFME, and 34 com­
pounds with a total proportion of 91.91% were identified in the essential
oil extracted by HD. The major constituents detected in the essential oil
Z. Liu et al.
Fig. 6. Total ion chromatograms and the major constituents of C. camphora fruit peel essential oil extracted by SFME and HD. Insert: chemical structural formulas of
the main compounds and their corresponding relative percentages in the essential oil extracted by SFME and HD.
extracted by SFME were similar to those in the essential oil extracted by
HD. The main components of the C. camphora fruit peel essential oil
using the SFME method were methyleugenol (50.52%), safrole
(13.42%), and eucalyptol (5.28%). For HD, the main constituents of the
essential oil were methyleugenol (37.71%), eucalyptol (10.12%), and
safrole (6.05%).
Higher amounts of methyleugenol and safrole were present in the
essential oil obtained by SFME compared to HD, as shown in Fig. 6.
Previous studies reported that oxygenated compounds, rather than
sesquiterpene hydrocarbons, were the main components of essential oil-
produced aromas (Ferhat, Meklati, Smadja, & Chemat, 2006; Zhao et al.,
2019). In this study, essential oil extracted through the SFME method
had a higher proportion of oxygenated compounds and a lower pro­
portion of sesquiterpene hydrocarbons than HD. Two reasons explain
this result: oxygenated compounds can interact more actively with mi­
crowaves due to having a higher dipolar moment than monoterpene
hydrocarbons, and thus, they are more easily released from plant ma­
terials (Filly et al., 2014); the shorter heating time in SFME might pre­
vent or reduce the decomposition of oxygenated compounds induced by
thermal and hydrolytic reactions (Bendahou et al., 2008; Khalili,
Mazloomifar, Larijani, Tehrani, & Azar, 2018). These results agree with
other studies that extracted plant essential oil under microwave irradi­
ation. Bousbia et al. (2009) proposed a microwave hydrodiffusion and
gravity method to isolate rosemary essential oil and observed an in­
crease in oxygenated compounds (microwave hydrodiffusion and
gravity, 29.54%; HD method, 26.16%). Tigrine-Kordjani, Meklati,
Chemat, and Guezil (2012) also found that the SFME method favored the
enrichment of oxygenated compounds in the obtained essential oil.
Drinić, Pljevljakušić, Živković, Bigović, and Šavikin (2020) applied a
microwave-assisted extraction method to isolate O. vulgare L. spp. hirtum
essential oil, and the results suggested a higher content of oxygenated
compounds in the essential oil obtained by the microwave-assisted HD
method compared to HD.
3.5. Physical properties of essential oil
C. camphora fruit peel essential oil obtained by SFME and HD was
subjected to physical analysis focused on density and optical rotation at
20 ◦ C, and the results are presented in Table 4. No obvious differences
were found for the physical constants of essential oil as a function of the
8
LWT 153 (2022) 112549
extraction methods (SFME versus HD). The sensory evaluation demon­
strated that SFME better maintained the natural aroma of plant essential
oil than HD. Therefore, SFME is a good alternative for the separation of
essential oil from C. camphora fruit peel.
3.6. SEM morphologies
SEM analysis was performed to investigate the physical changes of
peel treated with HD and SFME compared to the micrograph of the
untreated C. camphora fruit peel. Fig. 7a shows that the cells of the
untreated samples were smooth and intact. However, varying degrees of
physical destruction can be seen after extraction by SFME for 22 min
(Fig. 7b) and HD for 4 h (Fig. 7c). Fig. 7c shows that C. camphora fruit
peel became atrophic and appeared wrinkled after extraction by HD.
However, after extraction by the SFME method, the cells of C. camphora
fruit peel were greatly disrupted and wrinkled and appeared vacuous
upon release of the essential oil. In conventional HD, heat transfer was
only conduction and convection; in SFME, microwave irradiation could
cause a sudden increase in temperature as energy was absorbed by the in
situ water of the C. camphora fruit peel; as the water undergoes a phase
change and becomes steam, it increases the pressure inside the plant
cells, resulting in cell swelling and dramatic disruption of the cell walls.
Similar phenomena were also observed by Chen, Hu, Yao, and Liang
(2016) and Benmoussa et al. (2019) after isolation of the essential oils by
SFME from pomelo peel and the seeds of Foeniculum vulgare Mill.,
respectively. In summary, the SFME method was confirmed to be
quicker and more effective in separating C. camphora fruit peel essential
oil.
3.7. Environmental impacts of SFME and HD
The environmental impacts of SFME and HD with respect to elec­
tricity consumption, amount of CO2 released, and water consumption
are summarized in Table 3. SFME showed less environmental impact
than conventional HD with regard to electricity consumption (0.16 kW h
versus 4 kW h), CO2 release amount (128 g versus 3200 g), and amount
of wastewater (50 mL/g essential oil versus 722 mL/g essential oil).
These data show that SFME has great potential as a potential alternative
to conventional essential oil extraction methods. The results clearly
demonstrated that SFME has a better outcome than HD with respect to
Z. Liu et al. LWT 153 (2022) 112549

Table 3
Chemical composition of essential oil from C. camphora fruit peel by GC-MS analysis.
No.a Compounds Retention time (min) CAS number Molecular formula Relative peak area (%) RIb Identification

SFME HD

1 α-Pinene 7.01 2437-95-8 C10H16 0.08 0.71 917 RIc, MSd

2 β-Pinene 8.00 18172-67-3 C10H16 0.25 0.99 964 RI, MS
3 Sabinene 8.08 3387-41-5 C10H16 0.11 0.48 969 RI, MS
4 α-Myrcene 8.38 1686-30-2 C10H16 0.20 0.56 986 RI, MS
5 Octanal 8.64 0124-13-0 C8H16O 0.09 ND 993 RI, MS
6 α-Phellandrene 8.71 0099-83-2 C10H16 0.50 0.72 996 RI, MS
7 2-Carene 8.98 554-61-0 C10H16 NDe 0.67 1001 RI, MS
8 β-Cymene 9.15 0535-77-3 C10H14 0.09 ND 1031 RI, MS
9 D-Limonene 9.25 5989-27-5 C10H16 3.05 7.58 1035 RI, MS
10 Eucalyptol 9.31 0470-82-6 C10H18O 5.28 10.12 1038 RI, MS
11 α-Ocimene 9.63 0502-99-8 C10H16 1.82 0.93 1046 RI, MS
12 Terpinolene 10.47 0586-62-9 C10H16 0.15 1.32 1067 RI, MS
13 Linalol 10.65 0078-70-6 C10H18O 3.64 1.31 1090 RI, MS
14 Camphor 11.58 0076-22-2 C10H16O 6.23 1.26 1127 RI, MS
15 Citronellal 11.66 0106-23-0 C10H18O 0.30 0.17 1148 RI, MS
16 Isopulegol 11.81 0089-79-2 C10H18O 0.11 ND 1156 RI, MS
17 endo-Borneol 12.01 0507-70-0 C10H18O 0.27 3.80 1160 RI, MS
18 4-Terpineol 12.25 0562-74-3 C10H18O 0.45 1.10 1169 RI, MS
19 α-Terpieol 12.54 10482-56-1 C10H18O 1.79 2.63 1187 RI, MS
20 Estragole 12.69 0140-67-0 C10H12O 0.28 ND 1193 RI, MS
21 Citronellol 13.36 0106-22-9 C10H20O 0.45 0.61 1259 RI, MS
22 Geranial 13.75 0141-27-5 C10H16O 0.57 0.18 1269 RI, MS
23 β-Citral 14.61 0106-26-3 C10H16O 0.49 ND 1276 RI, MS
24 Safrole 15.33 0094-59-7 C10H10O2 13.42 6.05 1283 RI, MS
25 Citronellol acetate 17.37 0150-84-5 C13H24O2 0.36 0.68 1326 RI, MS
26 n-Decanoic acid 17.76 0334-48-5 C12H20O2 ND 0.26 1387 RI, MS
27 Geranyl acetate 18.21 0105-87-3 C12H20O2 0.98 1.26 1357 RI, MS
28 Methyleugenol 18.83 0093-15-2 C11H14O2 50.52 37.71 1364 RI, MS
29 Caryophyllene 19.24 0087-44-5 C15H24 0.43 1.02 1417 RI, MS
30 Humulene 19.97 6753-98-6 C15H24 0.39 0.60 1456 RI, MS
31 Muurolene 20.37 10208-80-7 C15H24 0.52 0.25 1457 RI, MS
32 Isohomogenol 20.67 0093-16-3 C11H14O2 1.70 2.27 1462 RI, MS
33 Chamigren 20.77 18431-82-8 C15H24 0.67 1.06 1472 RI, MS
34 δ-Cadinene 21.22 0483-76-1 C15H24 0.19 0.40 1493 RI, MS
35 Elemicin 21.67 0487-11-6 C15H16O3 0.16 0.25 1552 RI, MS
36 D-Nerolidol 21.81 0142-50-7 C15H26O 1.47 3.86 1565 RI, MS
37 Epiglobulol 22.52 88728-58-9 C15H26O ND 0.20 1608 RI, MS
38 τ-Muurolol 23.06 19912-62-0 C15H26O ND 0.22 1620 RI, MS
39 Cubenol 23.27 51371-47-2 C15H26O 0.18 0.68 1642 RI, MS
Total (%) 97.19 91.91
Oxygenated compounds (%) 88.74 74.62
Sesquiterpene hydrocarbons (%) 8.36 17.29
Others (%) 0.09 0
Extraction time (min) 24 240
Electric consumption (kW h) 0.16 4
RACO2 (g) 128 3200
Wastewater (mL/g essential oil) 50 722
a
Compounds listed in order of elution from HP-5 MS capillary column.
b
Retention indices relative to C11–C21 n-alkanes on HP-5 MS capillary column.
c
Tentative identification by comparison with RI on HP-5 MS capillary column with literature data.
d
Confirmed by comparison with mass data obtained from NIST05 mass spectra library.
e
ND = not detected.

the amount of CO2 released and wastewater to extract 1 g of the

Table 4
C. camphora fruit peel essential oil. Herein, SFME was proven to be an
Yield and physical properties of C. camphora fruit peel essential oil obtained by
economical and eco-friendly technique in the arena of green extraction
SFME and HD.
of plant essential oils.
SFME HD

Yield (mg/ 80.35 ± 1.88 75.19 ± 1.45 4. Conclusion

g)
Density (g/ 0.93 ± 0.02 0.90 ± 0.03
The SFME process was optimized with the BBD of RSM to achieve the
mL)
Optical 0 0 maximum yield of C. camphora fruit peel essential oil. The optimum
rotation SFME conditions with an actual yield of 80.35 ± 1.88 mg/g obtained
(◦ ) from BBD were a moisture content of 76%, microwave irradiation power
Aspect Liquid movable Liquid movable
of 420 W, and microwave irradiation time of 22 min. SFME performed
Colour Pale yellow Pale yellow
Odour Fresh, light, and freshly Freshly camphorated and boiled better than conventional HD with a much higher yield, shorter extrac­
camphorated odour, closed to odour, different from fresh fruit tion time and lower environmental impact. GC–MS results revealed that
fresh fruit peel peel C. camphora fruit peel essential oil obtained by SFME possessed better
quality than HD, as verified by the higher proportions of oxygen

9
Z. Liu et al.
Fig. 7. SEM morphologies of untreated C. camphora fruit peel (a), C. camphora
fruit peel after extraction by SFME (b), and after extraction by HD (c).
compounds. Physical analysis demonstrated found no obvious difference
in essential oil obtained by SFME and HD. SEM micrographs further
confirmed the effectiveness of SFME for the isolation of C. camphora fruit
peel essential oil. Therefore, SFME has promising prospects as an effi­
cient and green technique for isolating essential oil from plant materials.
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.
10
LWT 153 (2022) 112549
CRediT authorship contribution statement
Zaizhi Liu: Conceptualization, Funding acquisition, Supervision.
Hualan Li: Investigation, Data curation, Writing – original draft. Zheng
Zhu: Investigation, Data curation, Writing – original draft. Dai Huang:
Data curation, Methodology, Writing – original draft. Yanlong Qi:
Methodology, Data curation, Writing – review & editing. Chunhui Ma:
Software, Visualization, Validation, Methodology. Zhengrong Zou:
Visualization, Methodology, Funding acquisition. Hiyan Ni: Conceptu­
alization, Writing – review & editing, Supervision.
Declaration of competing interest
The authors declare that there is no conflict of interests regarding the
publication of this paper.
Acknowledgement
The authors thank the financial supports by Natural Science Foun­
dation of Jiangxi Province (20202BAB213024) and National Natural
Science Foundation of China (31860189 and 31760099).
References
Abdulrahman, A. (2021). Modeling and optimization of dynamic viscosity of copper
nanoparticles dispersed in gear oil using response surface methodology. Materials
Today: Proceedings, 42, 771–775.
Agu, C., Menkiti, M., Kadurumba, C., & Menkiti, N. (2015). Process parameter
optimization for transformer oil extraction from Terminalia catappa seed using
response surface methodology. Journal of the Chinese Advanced Materials Society, 3,
328–344.
Bajalan, I., Rouzbahani, R., Pirbalouti, A. G., & Maggi, F. (2018). Quali-quantitative
variation of essential oil from Iranian rosemary (Rosmarinus offcinalis L.) accessions
according to environmental factors. Journal of Essential Oil Research, 30, 16–20.
Bakkali, F., Averbeck, S., Averbeck, D., & Idaomar, M. (2008). Biological effects of
essential oils – a review. Food and Chemical Toxicology, 46, 446–475.
Bayramoglu, B., Sahin, S., & Sumnu, G. (2008). Solvent-free microwave extraction of
essential oil from oregano. Journal of Food Engineering, 88, 535–540.
Belhachat, D., Mekimene, L., Belhachat, M., Ferradji, A., & Aid, F. (2018). Application of
response surface methodology to optimize the extraction of essential oil from ripe
berries of Pistacia lentiscus using ultrasonic pretreatment. Journal of Applied Research
on Medicinal and Aromatic Plants, 9, 132–140.
Bendahou, M., Muselli, A., Grignon-Dubois, M., Benyoucef, M., Desjobert, J.-M.,
Bernardini, A.-F., et al. (2008). Antimicrobial activity and chemical composition of
Origanum glandulosum Desf. essential oil and extract obtained by microwave
extraction Comparison with hydrodistillation. Food Chemistry, 106, 132–139.
Benmoussa, H., Elfalleh, W., He, S., Romdhane, M., Benhamou, A., & Chawech, R.
(2018). Microwave hydrodiffusion and gravity for rapid extraction of essential oil
from Tunisian cumin (Cuminum cyminum L.) seeds: Optimization by response surface
methodology. Industrial Crops and Products, 124, 633–642.
Benmoussa, H., Farhat, A., Romdhane, M., & Bouajila, J. (2019). Enhanced solvent-free
microwave extraction of Foeniculum vulgare Mill. essential oil seeds using double
walled reactor. Arabin Journal of Chemistry, 12, 3863–3870.
Boukroufa, M., Boutekedjiret, C., Petigny, L., Rakotomanomana, N., & Chemat, F. (2015).
Bio-refinery of orange peels waste: A new concept based on integrated green and
solvent free extraction processes using ultrasound and microwave techniques to
obtain essential oil, polyphenols and pectin. Ultrasonics Sonochemistry, 24, 72–79.
Bousbia, N., Vian, M. A., Ferhat, M. A., Petitcolas, E., Meklati, B. Y., & Chemat, F. (2009).
Comparison of two isolation methods for essential oil from rosemary leaves:
Hydrodistillation and microwave hydrodiffusion and gravity. Food Chemistry, 114,
355–362.
Cassel, E., Vargas, R. M. F., Martinez, N., Lorenzo, D., & Dellacassa, E. (2009). Steam
distillation modeling for essential oil extraction process. Industrial Crops and
Products, 29(1), 171–176.
Chen, Q., Hu, Z., Yao, F. Y., & Liang, H. (2016). Study of two-stage microwave extraction
of essential oil and pectin from pomelo peels. Lebensmittel-Wissenschaft und
-Technologie- Food Science and Technology, 66, 538–545.
Chouhan, K. B. S., Tandey, R., Sen, K. K., Mehta, R., & Mandal, V. (2019). Critical
analysis of microwave hydrodiffusion and gravity as a green tool for extraction of
essential oils: Time to replace traditional distillation. Trends in Food Science &
Technology, 92, 12–21.
Cui, Q., Wang, L., Liu, J., Wang, H., Guo, N., Gu, C., et al. (2017). Rapid extraction of
Amomum tsao-ko essential oil and determination of its chemical composition,
antioxidant and antimicrobial activities. Journal of Chromatography B, 1061–1062,
364–371.
Drinić, Z., Pljevljakušić, D., Živković, J., Bigović, D., & Šavikin, K. (2020). Microwave-
assisted extraction of O. vulgare L. spp. hirtum essential oil: Comparison with
conventional hydro-distillation. Food and Bioproducts Processing, 120, 158–165.
Z. Liu et al.
Elik, A., Yanık, D. K., & Göğüş, F. (2020). Microwave-assisted extraction of carotenoids
from carrot juice processing waste using flaxseed oil as a solvent. LWT-Food Science
& Technology, 123, 109100.
Farhat, A., Benmoussa, H., Bachoual, R., Nasfi, Z., Elfalleh, W., Romdhane, M., et al.
(2017). Efficiency of the optimized microwave assisted extractions on the yield,
chemical composition and biological activities of Tunisian Rosmarinus officinalis L.
essential oil. Food and Bioproducts Processing, 105, 224–233.
Ferhat, M. A., Meklati, B. Y., Smadja, J., & Chemat, F. (2006). An improved microwave
Clevenger apparatus for distillation of essential oils from orange peel. Journal of
Chromatography A, 1112, 121–126.
Filly, A., Fernandez, X., Minuti, M., Visinoni, F., Cravotto, G., & Chemat, F. (2014).
Solvent-free microwave extraction of essential oil from aromatic herbs: From
laboratory to pilot and industrial scale. Food Chemistry, 150, 193–198.
Ghasemi Pirbalouti, A., Craker, L., & Alavi-Samani, S. M. (2018). Phytochemistry and
antioxidant activity of essential oils of condiment and spice plants from South
Western. Iranian Journal of Engineering and Applied Sciences, 13, 204–207.
Giacometti, J., Kovačević, D. B., Putnik, P., Gabrić, D., Bilušić, T., Krešić, G., et al.
(2018). Extraction of bioactive compounds and essential oils from mediterranean
herbs by conventional and green innovative techniques: A review. Food Research
International, 113, 245–262.
Guo, S., Geng, Z., Zhang, W., Liang, J., Wang, C., Deng, Z., et al. (2016). The chemical
composition of essential oils from Cinnamomum camphora and their insecticidal
activity against the stored product pests. International Journal of Molecular Sciences,
17, 1836.
Handayani, A. D., Sutrisno Indraswati, N., & Ismadji, S. (2008). Extraction of astaxanthin
from giant tiger (Panaeus monodon) shrimp waste using palm oil: Studies of
extraction kinetics and thermodynamic. Bioresource Technology, 99, 4414–4419.
He, F., Wang, W., Wu, M., Fang, Y., Wang, S., Yang, Y., et al. (2020). Antioxidant and
antibacterial activities of essential oil from Atractylodes lancea rhizomes. Industrial
Crops and Products, 153, 112552, 2020.
Jiang, H., Wang, J., Song, L., Cao, X., Yao, X., Tang, F., et al. (2016). Gc×Gc-tofms
analysis of essential oils composition from leaves, twigs and seeds of Cinnamomum
camphora l. presl and their insecticidal and repellent activities. Molecules, 21(4), 423.
Kapadiya, S. M., Parikh, J., & Desai, M. A. (2018). A greener approach towards isolating
clove oil from buds of Syzygium aromaticum using microwave radiation. Industrial
Crops and Products, 112, 626–632.
Khalili, G., Mazloomifar, A., Larijani, K., Tehrani, M. S., & Azar, P. A. (2018). Solvent-
free microwave extraction of essential oils from Thymus vulgaris L. and Melissa
officinalis L. Industrial Crops and Products, 119, 214–217.
Lee, H. J., Hyun, E. A., Yoon, W. J., Kim, B. H., Rhee, M. H., Kang, H. K., et al. (2006). In
vitro anti-inflammatory and anti-oxidative effects of Cinnamomum camphora
extracts. Journal of Ethnopharmacology, 103, 208–216.
Liu, Z., Chen, Z., Han, F., Kang, X., Gu, H., & Yang, L. (2016). Microwave-assisted method
for simultaneous hydrolysis and extraction in obtaining ellagic acid, gallic acid and
essential oil from Eucalyptus globulus leaves using Brönsted acidic ionic liquid [HO3S
(CH2)4mim]HSO4. Industrial Crops and Products, 81, 152–161.
Liu, Z., Deng, B., Li, S., & Zou, Z. (2018). Optimization of solvent-free microwave assisted
extraction of essential oil from Cinnamomum camphora leaves. Industrial Crops and
Products, 124, 353–362.
Liu, Z., Li, H., Cui, G., Wei, M., Zou, Z., & Ni, H. (2021). Efficient extraction of essential
oil from Cinnamomum burmannii leaves using enzymolysis pretreatment and followed
by microwave-assisted method. LWT - Food Science & Technology, 147, 111497.
Lucchesi, M. E., Chemat, F., & Smadja, J. (2004a). An original solvent free microwave
extraction of essential oils from spices. Flavour and Fragrance Journal, 19, 134–138.
Lucchesi, M. E., Chemat, F., & Smadja, J. (2004b). Solvent-free microwave extraction of
essential oil from aromatic herbs: Comparison with conventional hydro-distillation.
Journal of Chromatography A, 1043, 323–327.
Macedo, G. A., Santana, Á. L., Crawford, L. M., Wang, S. C., Dias, F. F. G., &
Bell, J. M. L. N. M. (2021). Integrated microwave- and enzyme-assisted extraction of
phenolic compounds from olive pomace. LWT-Food Science & Technology, 138,
110621.
Ma, C., Liu, T., Yang, L., Zu, Y., Chen, X., Zhang, L., et al. (2011). Ionic liquid-based
microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from
Schisandra chinensis Baill fruits. Journal of Chromatography A, 1218, 8573–8580.
Ma, C., Yang, L., Zu, Y., & Liu, T. (2012). Optimization of conditions of solvent-free
microwave extraction and study on antioxidant capacity of essential oil from
Schisandra chinensis (Turcz.) Baill. Food Chemistry, 134, 2532–2539.
Menichini, F., Conforti, F., Rigano, D., Formisano, C., Piozzi, F., & Senatore, F. (2009).
Phytochemical composition, anti-inflammatory and antitumour activities of four
Teucrium essential oils from Greece. Food Chemistry, 115, 679–686.
11
LWT 153 (2022) 112549
Meullemiestre, A., Kamal, I., Maache-Rezzoug, Z., Chemat, F., & Rezzoug, S. A. (2014).
Antioxidant activity and total phenolic content of oils extracted from Pinus pinaster
sawdust waste. Screening of different innovative isolation techniques. Waste and
Biomass Valorization, 5(2), 283–292.
Meziane, I. A. A., Maizi, N., Abatzoglou, N., & Benyoussef, E. H. (2020). Modelling and
optimization of energy consumption in essential oil extraction processes. Food and
Bioproducts Processing, 119, 373–389.
Michel, T., Destandau, E., & Elfakir, C. (2011). Evaluation of a simple and promising
method for extraction of antioxidants from sea buckthorn (Hippophaë rhamnoides L.)
berries: Pressurised solvent-free microwave assisted extraction. Food Chemistry, 126,
1380–1386.
Moazeni, M., Davari, A., Shabanzadeh, S., Akhtari, J., Saeedi, M., Mortyeza-Semnani, K.,
et al. (2021). In vitro antifungal activity of Thymus vulgaris essential oil
nanoemulsion. Journal of Herbal Medicine, 28, 100452.
Nabil, B., Vian- Abert, M., Ferhat, M. A., Petitcolas, E., Meklati, B. Y., & Chemat, F.
(2009). Comparison of two isolation methods for essential oil from rosemary leaves:
Hydrodistillation and microwave hydrodiffusion and gravity. Food Chemistry, 114,
355–362.
Patil, D. M., & Akamanchi, K. G. (2017). Microwave assisted process intensification and
kinetic modelling: Extraction of camptothecin from Nothapodytes nimmoniana plant.
Industrial Crops and Products, 98, 60–67.
Périno-Issartier, S., Ginies, C., Cravotto, G., & Chemat, F. (2013). A comparison of
essential oils obtained from lavandin via different extraction processes: Ultrasound,
microwave, turbohydrodistillation, steam and hydrodistillation. Journal of
Chromatography A, 1305, 41–47.
Pongsumpun, P., Iwamoto, S., & Siripatrawan, U. (2020). Response surface methodology
for optimization of cinnamon essential oil nanoemulsion with improved stability and
antifungal activity. Ultrasonics Sonochemistry, 60, 104604.
Qi, X., Li, T., Wei, Z., Guo, N., Luo, M., Wang, W., et al. (2014). Solvent-free microwave
extraction of essential oil from pigeon pea leaves [Cajanus cajan (L.) Millsp.] and
evaluation of its antimicrobial activity. Industrial Crops and Products, 58, 322–328.
Raut, J. S., & Karuppayil, S. M. (2014). A status review on the medicinal properties of
essential oils. Industrial Crops and Products, 62, 250–264.
Sodeifian, G., Sajadian, S. A., & Ardestani, N. S. (2017). Experimental optimization and
mathematical modeling of the supercritical fluid extraction of essential oil from
Eryngium billardieri: Application of simulated annealing (SA) algorithm. The Journal
of Supercritical Fluids, 127, 146–157.
Sokolova, A. S., Yarovaya, O. I., Shernyukov, A. V., Gatilov, Y. V., Razumova, Y. V.,
Zarubaev, V. V., et al. (2015). Discovery of a new class of antiviral compounds:
Camphor imine derivatives. European Journal of Medicinal Chemistry, 105, 263–273.
Sui, X., Liu, T., Ma, C., Yang, L., Zu, Y., Zhang, L., et al. (2012). Microwave irradiation to
pretreat rosemary (Rosmarinus officinalis L.) for maintaining antioxidant content
during storage and to extract essential oil simultaneously. Food Chemistry, 131,
1399–1405.
Tigrine-Kordjani, N., Meklati, B. Y., Chemat, F., & Guezil, F. Z. (2012). Kinetic
investigation of rosemary essential oil by two methods: Solvent-free microwave
extraction and hydrodistillation. Food Analytical Methods, 5, 596–603.
Vian, M. A., Fernandez, X., Visioni, F., & Chemat, F. (2008). Microwave hydrodiffusion
and gravity, a new technique for extraction of essential oils. Journal of
Chromatography A, 1190, 14–17.
Wang, W., Li, D., Huang, X., Yang, H., Qiu, Z., Zou, L., et al. (2019). Study on
antibacterial and quorum-sensing inhibition activities of Cinnamomum camphora leaf
essential oil. Molecules, 24, 3792.
Yan, X., Liang, S., Peng, T., Zhang, G., Zeng, Z., Yu, P., et al. (2020). Influence of phenolic
compounds on physicochemical and functional properties of protein isolate from
Cinnamomum camphora seed kernel. Food Hydrocolloids, 102, 105612.
Yanık, D. K. (2017). Alternative to traditional olive pomace oil extraction systems:
Microwave-assisted solvent extraction of oil from wet olive pomace. Lebensmittel-
Wissenschaft und -Technologie- Food Science and Technology, 77, 45–51.
Zarubaev, V. V., Garshinina, A. V., Tretiak, T. S., Fedorova, V. A., Shtro, A. A.,
Sokolova, A. S., et al. (2015). Broad range of inhibiting action of novel camphor-
based compound with anti-hemagglutinin activity against influenza viruses in vitro
and in vivo. Antiviral Research, 120, 126–133.
Zhang, G., Yan, X., Wu, S., Ma, M., Yu, P., Gong, D., et al. (2020). Ethanol extracts from
Cinnamomum camphora seed kernel: Potential bioactivities as affected by alkaline
hydrolysis and simulated gastrointestinal digestion. Food Research International, 137,
109363.
Zhao, Y., Wang, P., Zheng, W., Yu, G., Li, Z., She, Y., et al. (2019). Three-stage
microwave extraction of cumin (Cuminum cyminum L.) seed essential oil with natural
deep eutectic solvents. Industrial Crops and Products, 140, 111660.