Industrial Crops & Products 108 (2017) 716–721

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Industrial Crops & Products

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Green extraction of Cymbopogon citrus essential oil by solar energy MARK

a,⁎ b
Hsing Yuan Yen , Ya Chin Lin
a
Department of Greenergy Applications, Kao Yuan University, No. 1821, Zhongshan Rd., Lujhu Dist., Kaohsiung City, 82151, Taiwan
b
Institute of Cosmetology and Health Care, Kao Yuan University No. 1821, Zhongshan Rd., Lujhu Dist., Kaohsiung City, 82151, Taiwan

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

Keywords: The essential oil from Cymbopogon citrus is known for its use in various fields such as perfume, cosmetic,
Essential oil pharmaceutical and food industries. In this study, the merits of Cymbopogon citrus essential oil extracted by
Cymbopogon citrus both solar energy and hydro-distillation were evaluated, including the extraction yield and time, chemical
Solar energy composition (by gas-chromatography coupled with mass spectrometry, GC/MS), and antioxidant activity (DPPH
Hydro-distillation
free radical scavenging capacity). The energy consumption by these two methods was also investigated.
Antioxidant
The results show that the yields by solar energy extraction and hydro-distillation are nearly the same with
1.28% and 1.30%, respectively. The corresponding important compositions of citral (neral + geranial) are
66.53% and 60.78%, and DPPH free radical inhibitions in terms of IC50 are 33.52 mg/mL and 38.42 mg/mL.
That is, the antioxidant activity of the oil extracted by solar energy is better than that by hydro-distillation.
Moreover, hydro-distillation consumes 858 kWh of electricity per kg of essential oil whereas solar energy ex-
traction is free of any utility electricity. Thus, a completely sustainable green extraction method by solar energy
is a viable alternative to the traditional technique for extracting the Cymbopogon citrus essential oil.

1. Introduction
Cymbopogon citrus is a tropical perennial plant which yields aro-
matic essential oil. Its annual production is around 1000 tons from an
area of 16000 ha worldwide (Skaria et al., 2012) and its oil is regarded
as one of the most important essential oils being produced (Abdulazeez
et al., 2016). This oil can be utilized in various applications, such as
flavor and fragrance ingredients, perfumery, cosmetics, food additives,
and pharmaceutical and medicinal applications (Desai et al., 2014).
The Cymbopogon citrus essential oil is generally regarded as safe.
Its bioactivity is broad including antimicrobial (Bǒzik et al., 2017;
Liakos et al., 2016), antibacterial (Balakrishnan et al., 2014), antifungal
(Sarma et al., 2004), detoxifying activities (Tak et al., 2017), and even
in anticancer therapy (Thangam et al., 2014); these bioactivities have
been widely investigated. Further, its efficacy has also been proven to
treat a wide spectrum of health conditions physiologically as in ex-
cessive perspiration, flatulence, muscle aches, and scabies (Schaneberg
and Khan, 2002), and mentally as the anxiolytic, sedative or anticon-
vulsive agent (Blanco et al., 2009).
The quality of the essential oil is measured by the citral content
because it is the major active component found in Cymbopogon citrus
(Negrelle and Gomes, 2007). Traditionally, steam and hydro-distillation
techniques are commonly employed to extract the essential oil from the
Cymbopogon citrus leaves (Rao et al., 2016). Other methods for
extracting oils from Cymbopogon citrus are also available, such as by
supercitrical fluid or dense CO2 (Moncada et al., 2014; Carlson et al.,
2001), microwaves (Ajayi et al., 2016; Kumar et al., 2015; Desai and
Parikh, 2012), and solvents (Balakrishnan et al., 2014; Moncada et al.,
2014). All of the above extraction techniques have a high level of ef-
ficiency with high yield. However, supercritical fluid requires a high
pressure to condense CO2 and is dangerous; microwave heating con-
sumes a high electrical power. The volatile solvent causes environ-
mental pollution and is most harmful to the environment. If the se-
paration of solvent from the essential oil is not complete, the essential
oil will be contaminated by the solvent odor.
Moncada et al. revealed that the essential oil extracted from water
distillation is the lowest in terms of the production cost, potential en-
vironmental impact, and carbon footprint as compared with the su-
percriticial fluid and solvent extractions (Moncada et al., 2014). How-
ever, the water distillation still consumes heat energy and a large
quantity of cooling water.
At present, solar energy has been successfully utilized for cooking
and generating steam and electricity. In contrast, the essential oil ex-
traction by using solar energy is relatively new in the postharvest
sector. As examples, Munir et al., developed a solar distillery based on
the Scheffler reflector for extracting many essential oils including
peppermint, rosemary, and cumin (Munir et al., 2014; Munir and
Hensel, 2010). Maiti et al. extracted the orange peel oil by solar hydro-

⁎
Corresponding author.
E-mail addresses: t50031@cc.kyu.edu.tw (H.Y. Yen), ariel83130@gmail.com (Y.C. Lin).

http://dx.doi.org/10.1016/j.indcrop.2017.07.039
Received 27 April 2017; Received in revised form 24 June 2017; Accepted 26 July 2017
0926-6690/ © 2017 Elsevier B.V. All rights reserved.
H.Y. Yen, Y.C. Lin Industrial Crops & Products 108 (2017) 716–721

distillation via a parabolic solar collector (Maiti et al., 2012). However,

all of these researches utilized solar energy to heat water to boil the
herbs; i.e., indirect utilization of solar energy for oil extraction.
To date, no studies have employed solar energy directly to extract
the essential oil without water and any solar energy conversion to re-
place the traditional extraction methods. Therefore, in this study, an
innovative technology of using solar energy tube for oil extraction was
investigated. The specific goal of this paper aimed at comparing the
yield, extraction time, chemical composition and antioxidant activity of
DPPH (2,2-diphenyl-1-picrylhydrazyl) free radical scavenging capacity
by hydro-distillation and solar energy tube extractions. The energy
consumption by these two methods was also evaluated for their energy
utilization efficiencies.

2. Material and methods

2.1. Plant materials

The leaves of Cymbopogon citrus were obtained from a farm located

in Meinong town, Southern Taiwan (22°89′51.4″N 120°31′09.4″E) with
the altitude of 45 m above sea level and an average temperature of
27 °C. The leaves were pretreated by the following steps as shown in
Fig. 1: (1) cleaning by RO water; (2) drying at room temperature in a
sieve for 48 h; (3) cutting to pieces of 2 ± 0.2 cm in size; (4) weighting
500 g each for hydro-distillation and solar energy extraction. The size
and weight selections were to conform to the dimensions of the solar
energy tube to be described in the following section.

2.2. Extraction equipment

2.2.1. Solar energy extraction apparatus

The solar energy extraction apparatus is shown in Fig. 2a and b for
the schematic and the actual set-up, respectively. Its components
mainly consist of a solar energy tube, a sun light shade, a solar cell, a
battery, a temperature controller, and an essential oil collection unit.
These components were installed on a self-made right angle triangular
wooden frame of 160 cm (base) by 130 cm (height) by 70 cm (width) in
size as shown in Fig. 2b. The hypotenuse of the right angle was 206 cm.
The solar energy tube (SEP-360, Epoch Energy Technology Corp.,
Taiwan) was a vacuum type with the inner and outer diameters of
43 mm and 57 mm, respectively; the length was 235 cm. These tube
dimensions were the reasons for the leaves being 2 ± 0.2 cm in size Fig. 2. Experimental setup of the solar energy apparatus.
and 500 g in weight.
The experiments were carried out from AM 11:00 to PM 2:00 in The extraction temperature was controlled to 100 ± 5 °C by the
October, 2016 since October was a non-rainy month in southern temperature controller to regulate the sunlight intensity via the sunlight
Taiwan. During this time period, the outdoor temperature was about shade using the extraction temperature measured by a K-type thermo-
27–29 °C and the sun light intensity was about 920–980 W/m2. The couple. Because the thermal energy for decomposition was a radiation
solar energy tube was wholly filled with the leaves to facilitate oil type, no hot spot was observed inside the solar energy tube. The es-
collection. No water was added for the extraction. Hence, the essential sential oil collection unit included a collection bottle which was put
oils were obtained by thermal decomposition of the leaves by solar inside a cooling tank of temperature about 4 ± 0.5 °C. The cooling
energy alone.

Fig. 1. The experimental procedure of Cymbopogon

citrus essential oil extraction.

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H.Y. Yen, Y.C. Lin Industrial Crops & Products 108 (2017) 716–721

7.0
500 g in weight was placed in a flask containing 1500 mL of deionized
water and was hydro-distilled up to 3 h. The working power of 470 W
Cumulative essential oil yield (g)

6.0
was supplied for the heating mantle and that of 1760 W for the cooling
5.0 recirculation module under atmospheric pressure.

4.0
2.3. Analysis of sample
Hydro-distillation
3.0
2.3.1. Extraction yield
Solar energy
2.0 The mass of the extracted essential oil was measured by an analytic
balance with 0.0001 g in precision (Shimadzu, model AUW-D 220,
1.0
Japan). The essential oil was collected and stored in a sealed vial at 4 °C
0.0 prior to analysis and the moisture was removed by anhydrous sodium
0 30 60 90 120 150 180 sulphate (Merck, Germany). The essential oil yield (w/w) was calcu-
Time (min) lated according to Eq. (1).
(a) Cumulative yields weight ofessential oil collected (g )
Extraction yield(%) = × 100
initial weight of thefresh leaves (g ) (1)
0.143
0.14

2.3.2. Gas chromatography mass spectrometry (GC/MS) analysis

Essential oil yield rate (g/min)

0.12
Hydro-distillation The GC–MS analysis was performed in a Shimadzu GC–MS QP2010
0.096 system (Shimadzu, Japan), equipped with a DB-5 MS capillary column
0.10
Solar energy crosslinked with 5% Phenyl-methylpolysiloxane (30 m × 0.25 mm i.d.,
0.08 film thickness 0.25 μm; Agilent Tachnologies, J & W Scientific, CA,
U.S.A.). The oven temperature for separation was initially set to 50 °C,
0.06 then increased to 270 °C at the rate of 6 °C/min, and held at 270 °C for
0.049
0.037 0.035
10 min. The injection port temperature was set to 250 °C (injection
0.04
0.028
0.024 volume 1 μL with the split ratio of 100: 1). Helium, at the constant flow
0.02 rate of 0.73 mL/min, was the carrier gas. The mass spectra were re-
0.009
0.006 0.002 corded in the electron impact mode at 70 eV and scanned in the range
0.00 from 50 ∼700 m/z.
0-30 30-60 60-90 90-120 120-150 150-180 In addition, chemical compositions of the Cymbopogon citrus es-
(Time, min) sential oil were analyzed by comparing the relative retention indexes of
(b) Yield rates GC peaks with the indexes generated by fusing saturated n-alkanes (C8-
C23, plly Science Inc., Niles, USA) and by comparing of the mass spectra
Fig. 3. Cumulative and rate yields of Cymbopogon citrus essential oils.
of the peaks with the mass spectra reported and stored in National
Institute of Standards and Technology(NIST) and Wiley
condition was maintained by a thermoelectric cooler. The needed (Flavour & Fragrance Natural & Synthetic Compounds, FFNSC 1.2lib).
electricity for both shade and cooling control requirements was pro-
vided by a battery of 12 V/14 Ah which was charged by an 8W/18 V 2.3.3. Free radical scavenging activity
solar panel with the dimensions of 340 mm in length, 240 mm in width, The effect of essential oil extracts on DPPH degradation was mea-
and 25 mm in thickness. sured according to the method of previous studies (Noumi et al., 2011;
Ud-Daula et al., 2016; Luís et al., 2016). Samples of different con-
2.2.2. Hydro-distillation centrations were prepared in pure methanol (Merck, Germany); after
The hydro-distillation procedure was carried out with a conven- that, 2 mL of each of them was added to 0.5 mL of 0.2 mmol/L (v/v)
tional Clevenger apparatus. The pre-treated Cymbopogon citrus of DPPH solution (Sigma-Aldrich, USA); the mixture was left at room

Table 1
Major compositions of the Cymbopogon citrus essential oils.

Compound Category R. timea M. wt.b M. fc Area (%)

Hydro- distillation Solar Energy

6-Methyl heptane-2-one terpenes 8.073 126 C8H14O – 2.99

Myrcene monoterpenes 8.158 136 C10H16 12.41 10.47
Linalool monoterpenol 11.144 154 C10 H18O 0.82 2.25
Limonene oxide cyclic oxides 12.675 152 C10H16O 1.55 1.2
Verbenol monoterpenes 13.160 152 C10H16O 4.19 3.21
Caryophyllene oxide cyclic oxides 13.367 220 C15 H24 O 4.2 3.78
Neral terpenoids 14.825 152 C10H16O 26.68 29.72
Geraniol monoterpenol 15.596 154 C10 H18O 4.01 4.55
Geranial terpenoids 15.596 152 C10H16O 34.1 36.63
Geranyl acetate monoterpenes 17.981 196 C12 H20 O2 0.84 2.66
Citrald terpenoids 60.78 66.53

a
Rt: Retention time (min).
b
M. wt: Molecular weight.
c
M. f.: Molecular formula.
d
ctral(%) = neral (%) + geranial(%).

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H.Y. Yen, Y.C. Lin Industrial Crops & Products 108 (2017) 716–721

Fig. 4. Representative GC/MS spectrum of Cymbopogon citrus es-

sential oils.

temperature for 30 min. Then, the absorbance of the mixtures was blank (methanol), respectively. The concentration of essential oil that
measured at 517 nm (three replicates per treatment) by using a spec- reduced the absorption of DPPH solution by 50% (IC50, i.e. the con-
trophotometer (Hitachi U-2001, Japan) coupled with a computer for centration providing 50% of inhibition) was calculated from the cali-
data calculation. The DPPH radical scavenging ability of the essential bration curve (Majouli et al., 2016; Kanatt et al., 2014; Harkat-Madouri
oil was calculated according Eq. (2) et al., 2015).
(A0 − At )
DPPH scavenging activity(%) = × 100 2.4. Statistical analysis
A0 (2)
where At and A0 are the absorbance values of the sample and the The results are given in average ± standard deviation of triplicate

719
H.Y. Yen, Y.C. Lin
70
60
DPPH scavenging activity (%)
50
40
30
Hydro-disƟllaƟon
20
Solar Energy
10
0 concentrations from 5 to 60 mg/mL. The percentages of the scavenging
0 10 20 30 40 50 60
Essential oil concentration (mg/mL)
Fig. 5. DPPH scavenging activity of the Cymbopogon citrus essential oils.
for each sample. The IC50 values of DPPH were calculated by linear
regression analysis. The data were subjected to ANOVA and statistical
analyses were performed with SPSS (SPSS v.17). The results show that p
values were < 0.05; i.e., significant.
3. Results and discussion
3.1. Extraction yield of essential oils
The cumulative and rate of the essential oil yields are shown in
Fig. 3a and b, respectively. The results show that the maximum yield
rates of both hydro-distillation and solar energy extractions occurred at
0–30 min with the corresponding values of 0.143 g/min and 0.096 g/
min, respectively. There was no essential oil yield after 120 min by
hydro-distillation; whereas, there were still a few yields for
120–180 min by solar energy extraction. In addition, the yield rate of
hydro-distillation was higher than that of solar energy extraction before
60 min; the reverse was true after 60 min. The reason behind this dif-
ference is that water in the flask was heated more quickly and uni-
formly throughout the flask while the Cymbopogon citrus leaves were
being boiled. In contrast, the leaves in the solar energy tube could not
be heated as uniformly and fully as those in water due to lack of fluid
stirring. However, despite of their difference in yield rate, their final
cumulative yields are approximately the same; they are 6.498 g
(1.30%) and 6.375 g (1.28%) for hydro-distillation and solar energy
extraction, respectively.
3.2. Chemical components of cymbopogon citrus essential oil
Due to the complex compositions of the Cymbopogon citrus essen-
tial oil, only the major and important constituents are presented in this
study for clarification. The percentages of the major compounds of the
essential oil are shown in Table 1 and depicted in Fig. 4a and b. The
results show that, for both extraction methods, they are nearly the same
except 6-Methyl heptane-2-one. This latter compound is also found in
the Cymbopogon citrus essential oil extracted by dense carbon dioxide
(Carlson et al., 2001), and by re-distillation and solvent extraction of
Cymbopogon citrus hydrosol (Rao et al., 2016).
On the other hand, the percentages of myrcene, limonene oxide,
verbenol, caryophyllene oxide extracted by hydro-distillation are
slightly higher than those by solar energy extraction. However, the
important compositions of linalool (2.25%), neral (29.72%), geraniol
(4.55%), geranial (36.63), geranyl acetate (2.66%) by solar energy
extraction are all higher than those by hydro-distillation extraction. In
particular, the percentages of citral (neral + geranial) are 66.53% and
60.78% for solar energy and hydro-distillation extractions, respectively.
Industrial Crops & Products 108 (2017) 716–721
In general, the Cymbopogon citrus essential oil is characterized by the
concentration level of citral (Tovar et al., 2010) as it has been used in
traditional and oriental folk medicines for millennia (Moyler, 2009).
Moreover, the main active ingredients of citral, neral, and geraniol have
been shown to be effective in inactivating food-borne pathogens
(Abdulazeez et al., 2016; Desai et al., 2014; Mohamed Hanaa et al.,
2012). Hence, solar energy extraction performs better in this aspect.
3.3. Antioxidant activity
Fig. 5 shows the results of the scavenging effect of the Cymbopogon
citrus essential oils on the DPPH radical. It can be seen that the DPPH
scavenging capacity of the tested oils increased by increasing their
70 ability are from 12.3% to 54.2% and 13.1% to 58.4% for hydro-dis-
tillation and solar energy extraction, respectively. The corresponding
values of IC50 are 38.42 ± 0.6 mg/mL and 33.52 ± 0.8 mg/mL. The
IC50 of essential oil from solar energy extraction is somewhat lower
than that from hydro-distillation. As a lower value of IC50 corresponds
to a higher antioxidant activity (Harkat-Madouri et al., 2015), solar
energy performs slightly better in this regard.
3-4 Comparison of energy consumption
For hydro-distillation, both heating (470 W) and cooling (1760 W)
were needed. The process time was 2.5 h including 0.5 h of preheating/
precooling and 2 h of extraction as no more yields were produced
afterwards. Hence, its energy consumption calculated from Eq. (3) was
858 kWh per kg Cymbopogon citrus essential oil whereas solar energy
extraction was free of any utility energy. Thus, from the results de-
scribed above, it is clear that a completely green extraction method by
solar energy is a viable alternative to the traditional technique for ex-
tracting the essential oil from the Cymbopogon citrus.
470 + 1760
Energyconsumption(kWh/kg) = × 2.5 ÷ 6.498 × 1000
1000
= 858kWh/kg (3)
On the other hand, the disadvantages of using solar energy are
mainly the availability of solar energy (such as geographical conditions
and the possibility of rainy seasons) and the initial setup cost of the
solar energy tube, solar cell, battery, and controllers. Moreover, as solar
extraction was conducted outdoor, the collection bottles must be pro-
tected from sunlight by shading for avoiding degradation of the es-
sential oils.
4. Conclusion
In this study, the merits of the Cymbopogon citrus essential oil ex-
tracted by both solar energy and hydro-distillation were evaluated. The
key results are summarized as follows.
The extraction yields for both methods are similar. The percentage
of the most important composition of the essential oil, citral (neral
+ geranial), extracted by solar energy is higher than that by hydro-
distillation. Moreover, hydro-distillation consumes 858 kWh of elec-
tricity per kg of Cymbopogon citrus essential oil whereas solar energy
extraction is free of any utility electricity. Therefore, the essential oil
extracted by solar energy is a viable alternative to the traditional ex-
traction technique.
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