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Extraction of essential oil from cananga (Cananga odorata) using solvent-free microwave extraction: A preliminary study

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Today the production of cananga (Cananga odorata) oil still has the potential to be developed in Indonesia. But the extraction of essential oil from cananga flowers are still using conventional methods such as hydrodistillation, steam-hydrodistillation and steam distillation which takes a long time to produce oil with good quality. In this research the extraction of cananga oil is done using solvent-free microwave extraction (SFME) method. The optimum yield in the extraction of cananga oil using SFME method is 2.304%. The optimum yield is obtained on the operating conditions: microwave power of 380 W, feed to distiller (F/D) ratio of 0.05 g/mL and flower size of ±0.5 cm. Based on the results of the GC-MS analysis showed that the main components of cananga oil produced by SFME method were β-caryophyllene (16.855%), benzyl benzoate (14.326%), caryophyllene oxide (13.484%) and germacrene (10.692%). Additionally, from GC-MS analysis can be said that the cananga oil that has been extracted using SFME method offers the possibility for better reproduction of the natural aroma of the flower essential oil than that obtained using the conventional method.
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Vol. 10 | No. 1 |86-91 | January - March | 2017
ISSN: 0974-1496 | e-ISSN: 0976-0083 | CODEN: RJCABP
http://www.rasayanjournal.com
http://www.rasayanjournal.co.in
Rasayan J. Chem., 10(1), 86-91(2017)
http://dx.doi.org/10.7324/RJC.2017.1011562
EXTRACTION OF ESSENTIAL OIL FROM CANANGA
(Cananga odorata) USING SOLVENT-FREE MICROWAVE
EXTRACTION: A PRELIMINARY STUDY
M. Mahfud
*
, D.K.Y. Putri, I.E.P. Dewi and H.S. Kusuma
*
Department of Chemical Engineering, Faculty of Industrial Technology, Institut Teknologi
Sepuluh Nopember, Surabaya-60111, Indonesia
*E-mail: mahfud@chem-eng.its.ac.id; heriseptyakusuma@gmail.com
ABSTRACT
Today the production of cananga (Cananga odorata) oil still has the potential to be developed in Indonesia. But the
extraction of essential oil from cananga flowers are still using conventional methods such as hydrodistillation, steam-
hydrodistillation and steam distillation which takes a long time to produce oil with good quality. In this research the
extraction of cananga oil is done using solvent-free microwave extraction (SFME) method. The optimum yield in the
extraction of cananga oil using SFME method is 2.304%. The optimum yield is obtained on the operating conditions:
microwave power of 380 W, feed to distiller (F/D) ratio of 0.05 g/mL and flower size of ±0.5 cm. Based on the results
of the GC-MS analysis showed that the main components of cananga oil produced by SFME method were β-
caryophyllene (16.855%), benzyl benzoate (14.326%), caryophyllene oxide (13.484%) and germacrene (10.692%).
Additionally, from GC-MS analysis can be said that the cananga oil that has been extracted using SFME method offers
the possibility for better reproduction of the natural aroma of the flower essential oil than that obtained using the
conventional method.
Keywords: Cananga odorata, cananga oil, solvent-free microwave extraction.
© RASĀYAN. All rights reserved
INTRODUCTION
Essential oil is one of an agro-industry export commodity that is potential to be a mainstay for Indonesia to
earn foreign exchange. The statistical data of world export-import show that the average growth of essential
oils and derivatives consumption is 5-10% per year. This increase was mainly driven by growing needs for
food flavoring industry, cosmetics industry, and fragrances. Essential oils which have been widely extracted
in Indonesia, among others, patchouli, clove, nutmeg, lemongrass, vetiver, eucalyptus oil, and others. While
there are some essential oils that are still potential to be developed such as cananga, basil, cardamom,
cinnamon, and others.
Cananga (Cananga odorata) is known for its flowers have a fragrant smell. In Java and Bali, cananga traded
by local residents as potpourri and sow flowers used in religious ceremonies. In addition, cananga is also
known as a medicinal plant, the leaves as a remedy for itch
1
, dried flowers for malaria drugs
2
, fresh flowers
for aroma therapy, as well as the bark as a remedy for ulceration. Essential oils contained in cananga flowers
is used as a fragrance ingredient. Cananga oil has quite high economic value in the world market. In addition
to economic value, cananga trees also have ecological value, where this trees can be used for slope stability
due to the type of roots are strong.
But today generally extraction process of essential oils from dried cananga flowers is still done using
conventional methods such as hydrodistillation, steam-hydrodistillation and steam distillation. The length
of time and still small yield obtained from conventional methods led to the need for the development of the
methods of essential oils extraction. One of the methods that have the potential to be used for extraction of
cananga oil is microwave-assisted extraction (MAE) methods.
3
MAE methods which now widely used,
among others, microwave-assisted hydrodistillation (MAHD), microwave steam distillation (MSD),
microwave steam diffusion (MSDf), and microwave hydro diffusion and gravity (MHG).
4,5
The advanced
development of MAE method is solvent-free microwave extraction (SFME) method.
6
This method has the
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EXTRACTION OF ESSENTIAL OIL FROM CANANGA M. Mahfud
et al.
advantages compared with previously mentioned methods such as having faster extraction rate, yield, and
also higher purity of extract because it does not require solvent so that does not contact with chemicals.
Therefore, in this research, the essential oil from dried cananga flowers extracted using SFME method. The
extraction using these methods is expected to obtain optimum yield and quality of cananga oil that can be
accepted in the market.
EXPERIMENTAL
Plant Material
Fresh cananga (Cananga odorata) flowers were collected from Pasuruan, East Java, Indonesia. The flowers
then were dried and stored at room temperature until required.
Solvent-Free Microwave Extraction (SFME) of Cananga Oil
In employing SFME, we used a domestic microwave oven (EMM-2007X, Electrolux, 20 L, maximum
delivered power of 800 W) with a wave frequency of 2450 MHz. In a typical SFME procedure performed
at atmospheric pressure, flower size of 0.5, 2.5 and 5.0 cm and feed to distiller (F/D) ratio of 0.05 g
mL
-1
were wetted before extraction by soaking in a certain proportion of distilled water for 30 min, and
then removal the excess distilled water. The wetted material was placed in a 1 L flask. The microwave oven
was operated at a power level of 100, 240 and 380 W for a period of 1 h. To remove water, the extracted
cananga oil were then dried over anhydrous sodium sulfate, weighed and stored in amber vials at 4
o
C until
they were used for analysis. The yield of cananga oil was calculated as follows:
  
   
Fig.-1: Schematic representation of solvent-free microwave extraction (SFME) method for extraction of cananga oil
Chemical Analysis of Essential Oil Components
Essential oils components were determined on the basis of gas chromatography (GC) retention time on
fused silica capillary column, by comparison of their mass fragmentation pattern with literature reports and
by computer matching with standard spectra.
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EXTRACTION OF ESSENTIAL OIL FROM CANANGA M. Mahfud
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RESULTS AND DISCUSSION
The Extraction of Cananga Oil using Solvent-Free Microwave Extraction (SFME) Method
In the extraction process of cananga oil, the determination of the optimal microwave power for the
extraction process is very important because microwave power also affects the temperature during the
extraction process. Figure 2 shows the effect of various microwave power to temperature. The high
microwave power was used so that the polar molecules in the material rotate faster when exposed to
microwave radiation (motion oscillation and collide each other) and generate heat energy which is detected
by the increase in temperature. The higher the microwave power used, the higher the generated energy will
be. This can be described using the following equation:
 
, where E = Q = m.Cp.T
So, it can be seen that P E T (power is proportional to the energy and the increase of temperature).
3
In order to better understand this, the temperature profile for various microwave power that is used in the
extraction process of cananga oil can be seen in Figure-2.
Fig.-2: Temperature profile for various microwave power that is used in the extraction of cananga oil using solvent-
free microwave extraction (SFME) method
The rate of the temperature rise for each of the microwave power can be measured by determining the slope
of the linear section contained on the temperature profile.
7
From Figure 2, it can be seen that the rate of
temperature rise for each of the used microwave power in the extraction process is as follows: 100 W is
3.35
o
C/min; 240 W is 14.48
o
C/min, and 380 is 18.70
o
C/min.
From Figure 2, it can generally be seen that the most rapid microwave power to raise the temperature is
380 W. However, in the extraction process using SFME method, there are material characteristics that affect
the extraction process. The presence of the material characteristics may cause the extraction process of
cananga oil using SFME method with the microwave power of 380 W not necessarily produce the optimum
yield.
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EXTRACTION OF ESSENTIAL OIL FROM CANANGA M. Mahfud
et al.
Fig.-3: The effect of microwave power to yield of cananga oil (F/D ratio of 0.05 g/mL)
In general, it can be seen that the optimum microwave power to optimally produce cananga oil yield for
dried material is 380 W. The effect of the microwave power to yield of cananga oil can be seen in Fig.-3.
In this research was obtained optimum yield is 2.304% on the operating conditions: microwave power of
380 W, F/D ratio of 0.05 g/mL and flower size of ±0.5 cm. The cananga oil yield obtained in the extraction
using SFME method is higher when compared to the extraction using water-steam distillation method that
has been done by Megawati and Saputra (2012)
8
. In the extraction using water-steam distillation for 8 hours
obtained cananga oil yield is 0.936%. So it can be said that the extraction of cananga oil using SFME
method is faster when compared with water-steam distillation method.
GC-MS Analysis
To find out the components contained in cananga oil analysis is done using Gas Chromatography-Mass
Spectrometry (GC-MS). The results of the GC-MS analysis can be seen from the obtained chromatogram
(Figure-4 ). From the chromatogram can be seen that in the cananga oil that has been extracted using SFME
method there are 63 components. Based on the results of GC-MS analysis also showed that the main
components of cananga oil produced by SFME method were β-caryophyllene (16.855%), benzyl benzoate
(14.326%), caryophyllene oxide (13.484%) and germacrene (10.692%). The results of the GC-MS analysis
for cananga oil that has been extracted by other methods showed different results. It can be seen from the
results of the GC-MS analysis for cananga oil that has been extracted using water-steam distillation method
that has been done by Megawati and Saputra (2012)
8
. The main components of cananga oil produced by
water-steam distillation method were trans-carryophyllene (39.03%), α-humulene (11.59%), α-
bergamotene (11.29%) and germacrene (10.94%).
The significant difference can be seen in the main components that have been extracted. Where in the
cananga oil that has been extracted using SFME method there are oxygenated components on its main
components. While in the cananga oil that has been extracted using water-steam distillation method there
is no presence of oxygenated components on its main components. In addition we need to know that the
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EXTRACTION OF ESSENTIAL OIL FROM CANANGA M. Mahfud
et al.
scent of essential oils is very affected by the amount of oxygenated components. The oxygenated
component is highly odoriferous, while the sesquiterpene hydrocarbon contributes only little to fragrance
produced. So based on the results of the GC-MS analysis that presented in Table-1 it can be said that the
cananga oil that has been extracted using SFME method offers the possibility for better reproduction of the
natural aroma of the flower essential oil than that obtained using water-steam distillation method.
Fig.-4: A chromatogram of cananga oil extracted using solvent-free microwave extraction (SFME) method
Vol. 10 | No. 1 |86-91 | January - March | 2017
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EXTRACTION OF ESSENTIAL OIL FROM CANANGA M. Mahfud
et al.
Tabel-1: Class of components contained in cananga oil
No Class of Components
Area (%)
SFME
(this research)
Water-steam distillation
(Megawati and Saputra,
2012)
1 Monoterpenes 0.448 0.00
2 Oxygeneted Monoterpenes 6.781 11.49
3 Sesquiterpenes 49.937 84.13
4 Oxygeneted Sesquiterpenes 17.619 1.39
5 Other Components 0.093 0.00
6 Other Oxygenated Components 25.121 2.98
Yield (%) 2.304 0.936
CONCLUSION
Solvent-free microwave extraction (SFME) method can be used for extraction of essential oils from dried
cananga flowers. The optimum yield in the extraction of cananga oil using SFME method is 2.304%. The
optimum yield is obtained on the operating conditions: microwave power of 380 W, feed to distiller (F/D)
ratio of 0.05 g/mL and flower size of 0.5 cm. Based on the results of the GC-MS analysis showed that the
main components of cananga oil produced by SFME method were β-caryophyllene (16.855%), benzyl
benzoate (14.326%), caryophyllene oxide (13.484%) and germacrene (10.692%). Additionally, from GC-
MS analysis can be said that the cananga oil that has been extracted using SFME method offers the
possibility for better reproduction of the natural aroma of the flower essential oil than that obtained using
the conventional method.
ACKNOWLEDGEMENT
This research project was financially supported by the Indonesia Endowment Fund for Education (Lembaga
Pengelola Dana Pendidikan/LPDP).
REFERENCES
1. L.H. Burkill, A Dictionary of the Economic Products of the Malay Peninsula, University Press, Oxford
(1935).
2. K. Heyne, Tumbuhan Berguna Indonesia IV (in Bahasa Indonesia), Badan Litbang Kehutanan, Jakarta
(1987).
3. H.S. Kusuma and M. Mahfud, RSC Advances, 7(3), 1336 (2017).
4. H.S. Kusuma and M. Mahfud, Journal of Applied Research on Medicinal and Aromatic Plants,
Articles in Press (2016). DOI: 10.1016/j.jarmap.2016.08.001
5. H.S. Kusuma and M. Mahfud, Journal of Applied Research on Medicinal and Aromatic Plants,
Articles in Press (2016). DOI: 10.1016/j.jarmap.2016.08.002
6. H. Kusuma, D. Putri, I. Dewi and M. Mahfud, Chemistry and Chemical Technology, 10(2), 213 (2016).
7. M.-T. Golmakani and M. Moayyedi, Food Science and Nutrition, 3(6), 506 (2015).
8. Megawati and S.W.D. Saputra, IOSR Journal of Engineering, 2(10), 5 (2012).
[RJC-1562/2017]
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Leaves of Pogostemon cablin were subjected to microwave-assisted hydrodistillation (MAHD) and solvent-free microwave extraction (SFME), respectively. A comparison was made between MAHD and SFME with the conventional hydrodistillation (HD) method in terms of effectiveness in the extraction of essential oil (EO). The microwave-assisted extraction methods offer important advantages over conventional alternatives, viz. shorter extraction times (66 min for MAHD and 45 min for SFME vs. 417 min for HD); almost equal yields (2.177% for MAHD and 2.374% for SFME vs. 2.622% for HD); lower relative electric consumption (1.509 kWh/g EO for MAHD and 0.417 kWh/g EO for SFME vs. 13.821 kWh/g EO for HD); and lower relative amounts of CO2 emissions (1.207 kg CO2/g EO for MAHD and 0.334 kg CO2/g EO for SFME vs. 11.056 kg CO2/g EO for HD). A mathematical model based on heat and mass transfer fundamentals is applied to correlate the experimental data. Higher yield results from higher extraction rates by microwaves and could be due to a synergy of two transfer phenomena: heat and mass acting in the same way. The results of this study suggest that MAHD and SFME can be termed as green technologies because of their less energy requirements per gram of essential oil extraction.
Article
Full-text available
Solvent-free microwave extraction (SFME) is proposed as a method for " green " extraction of edible essential oils extensively used in the fragrance, flavour, and pharmaceutical industries and also in aromatherapy. It is a combination of microwave heating and dry distillation, performed at atmospheric pressure without adding any solvent or water. Isolation and concentration of volatile compounds are performed by a single stage. Basil (Ocimum basilicum L.) was extracted with SFME at atmospheric pressure and 373 K for 30 min. The extracted compounds were removed from the aqueous extract by simple decantation, identified by gas chromatography– mass spectrometry (GC-MS). Hydrodistillation (HD) of basil was performed with 400 ml of water for 4.5 h for comparison of the results with those provided by the proposed method. SFME method offers important advantages over HD, viz. shorter extraction times (30 min vs. 4.5 h); better yields (0.13 % vs. 0.11 %); environmental impact (energy cost is appreciably higher for performing HD than that required for rapid SFME), cleaner features (as no residue generation and no water or solvent used); and provides a more valuable essential oil. SFME is a green technology and appears as a good alternative for the extraction of edible essential oils from aromatic plants used in aromatherapy and food industry.
Article
Dried and fresh peels of Citrus limon were subjected to microwave-assisted hydrodistillation (MAHD) and solvent-free microwave extraction (SFME), respectively. A comparison was made between MAHD and SFME with the conventional hydrodistillation (HD) method in terms of extraction kinetic, chemical composition, and antioxidant activity. Higher yield results from higher extraction rates by microwaves and could be due to a synergy of two transfer phenomena: mass and heat acting in the same way. Gas chromatography/mass spectrometry (GC/MS) analysis did not indicate any noticeable differences between the constituents of essential oils obtained by MAHD and SFME, in comparison with HD. Antioxidant analysis of the extracted essential oils indicated that microwave irradiation did not have adverse effects on the radical scavenging activity of the extracted essential oils. The results of this study suggest that MAHD and SFME can be termed as green technologies because of their less energy requirements per ml of essential oil extraction.
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