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Article in The Journal of microwave power and electromagnetic energy: a publication of the International Microwave Power Institute · January 2013
DOI: 10.1080/08327823.2013.11689846 · Source: PubMed
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Microwave-assisted Extraction of
Essential Oils from Herbs
Gabriel Abraham Cardoso-Ugarte, Gladys Paola Juárez-Becerra, María Elena Sosa-
Morales, Aurelio López-Malo
Departamento de Ingeniería Química, Alimentos y Ambiental, Universidad de las Américas
Puebla. Sta. Catarina Mártir, Cholula, Puebla 72820, México
INTRODUCTION
Microwaves are a form of non-ionizing electromagnetic energy at frequencies ranging
from 300 MHz to 300 GHz. This energy is transmitted as waves, which can penetrate in
biomaterials and interact with polar molecules into materials, such as water to generate heat
[Takeuchi et al., 2009]. Fast heating is the main advantage of microwaves; the application
in foods is performed at frequencies of 915 MHz at industrial scale and 2450 MHz in domestic
ovens [Routray and Orsat, 2012].
Due to economics and environmental issues, food and chemical industries are facing
the challenge of using new technologies in order to reduce energy consumption and CO2
emissions [Bousbia et al., 2009]. Separation technologies, such as extraction, distillation
and crystallization are promising areas of innovation which can promote the growth of
sustainable processes in the chemical and food industries [Perino-Issartier et al., 2010].
Application of microwaves in separation and extraction processes has shown to
reduce both extraction time and volume of solvent required, minimizing environmental
impact by emitting less CO2 in atmosphere [Lucchesi et al., 2004; Ferhat et al., 2006] and
consuming only a fraction of the energy used in conventional extraction methods such as
steam distillation, SD [Farhat et al., 2009]. Advances in microwave-assisted extraction
(MAE) have led in the development of various techniques such as compressed air microwave
distillation (CAMD), vacuum microwave obtained essential oil from Vicia herb using
hydro distillation (VMHD), microwave hydro and microwave distillations.
hydro distillation (MWHD), solvent-free Epazote (Chenopodium ambrosioides),
microwave extraction (SFME), microwave member of the family Chenopodiacea, is an
accelerated steam distillation (MASD), aromatic plant whose leaves have been used
microwave by hydro diffusion and gravity to cure influenza, pneumonia, typhoid and as
(MHG) [Perino-Issartier et al., 2010; Farhat vermifuge, they have shown anthelmintic and
et al., 2009]. analgesic properties so as to treat dysentery,
MAE is a current technology to extract stomachache and as a flavoring agent; its
biological materials and has been regarded essential oil has been used as antifungal,
as an important alternative in extraction nematicide and insecticide [Kumar et al.,
techniques because of its advantages which 2007]. Meanwhile, basil (Ocimum basilicum
mainly are: reduction of extraction time L.) belonging to Lamiaceae family is an
and solvents, selectivity, volumetric heating aromatic herb that has been widely used in
and controllable heating process. Various food as a flavoring agent and in perfumery
researches has shown the efficiency of MAE and pharmaceutical industries [Ijaz et al.,
in the extraction of different compounds 2008]. Evenly, in traditional medicine its
such as essential oils, fragrances, pigments, leaves and flowers have been used as remedy
antioxidants and other organic compounds as for digestive [Politeo et al., 2007; Ebrahim,
animal tissues, food and plants. In addition 2006] and respiratory diseases [Simon et al.,
of the reduction of time, solvent usage and 1999]. On the other hand, its essential oil
energy consumption, this process shows has insecticidal, nematicidal, fungistatic
even more benefits like a more effective and antimicrobial properties [Politeo et al.,
heating, faster energy transfer, size reduced 2007]. Additionally, its phenolic compounds
equipment, rapid onset of warming and and flavonoids have shown to be powerful
increased yields [Farhat et al., 2009]. antioxidants [Ijaz et al., 2008], free radical
The use of MAE in the isolation scavengers and metal chelators [Jayasinghe
of herbal essential oils is an interesting et al., 2003].
alternative that provides more effectiveness Therefore, the aim of this study was:
than other processes [Bousbia et al., 1) to determine the influence of three main
2009] as the conventional extraction of factors (amount of water, power and heating
essential oils of herbs and spices by steam time) in the MAE process of essential oils from
distillation. Several authors have used two herbs (basil and epazote) by applying a
microwave extraction techniques to obtain two-level factorial design in order to define
essential oils from herbs. Early reports its optimal extraction conditions, and
of MAE application to extract essential
oils were recorded in the 80’s [Letellier 2) to characterize and analyze the physical
and Budzinski, 1999]. Craverio et al. and chemical properties of the essential
[1989] compared this process with steam oils obtained by MAE to compare them with
distillation, the oils obtained from Lippia the essential oils obtained by SD in order to
sidoides leaves did not show qualitative establish MAE as an alternative method to
difference, but quantitative differences extract essential oil from herbs.
were observed. More recently, Mohammad-
Taghi et al. [2008] also compared these two MATERIALS AND METHODS
methods for obtaining essential oil from Raw material
Thymus vulgaris. Dragovic-Uzelac et al. Two different herbs were purchased
[2012] employed MAE to get polyphenols in a local market of Puebla in Mexico:
from wild sage, and Kahriman et al. [2012] basil (Ocimum basilicum L.), and epazote
(Chenopodium ambrosioides L.). The obtained. Vapors began to rise into the
leaves were separated and dried at room flask’s neck until reach the condenser where
temperature from which the essential oils they were cooled, the extracted liquid was
were extracted. The obtained essential oils received into a trap; the essential oils were
were kept into closed amber vials for their recovered and its volume was determined
further analysis. using a micropipette, the remaining water
in oils was removed by adding anhydrous
Microwave-assisted extraction sodium sulfate. Yields were calculated as
The extraction of the essential oils was percentage (volume of extracted oil per
performed using a domestic microwave oven weight of dried herb). The oil was placed
(600 W, Daewoo, China). From preliminary into screw cap amber test tubes and stored
tests, it was found that low power levels under refrigeration until its analysis.
(from 20 to 60% of the maximum power)
resulted in long extraction times, while high Steam distillation extraction
powers slightly burned the leaves. The oven For comparison, steam distillation
was adapted (Figure 1) as follows: 100 g extractions of the essential oils were carried
of sample (dried leaves) were placed in a out in a steam distillation apparatus which
1000 mL flat-bottomed flask and the solvent consists of the following accessories: electric
amount (distilled water) to analyze was hot plate, Pyrex glass flask, a 500 mL beaker
added (400 or 500 mL); the flask containing for the reception of the distillate, distillation
the sample was introduced to the microwave head, condenser adapted to the coolant,
oven and adjusted to a condenser connected clamps, hoses and insulating material. For
to a cold water recirculation system; the the extraction process, 1500 mL of distilled
microwave oven was turned on and the water were added to the container with some
desired conditions of time (20 or 30 min) and boiling beads and placing the flask on the hot
power (70 or 80%) were set to allow heating plate; subsequently, 150 g of fractionated
of the herb-water blend and the consequent dried herb were placed in the upper flask,
generation of vapors. No stirring or rotation around the flask an insulating material was
were possible within the flask, however, placed to prevent heat loss. The cooling
the amount of water allowed acceptable system was turned on to cool the water
convection and enough homogeneity was inside the condenser and the distillation
Figure 1. Schematic diagram of the microwave oven adaptation to perform MAE of essential oils from herbs.
process started by setting the hot plate to (1.5 mL/min) and the injector at 240 °C;
boil water. Generated vapors began to rise temperature in the column after an initial
toward the head of the distillation apparatus period is hold for 10 min at 60 °C, later is
until the condenser where it cools. increased every 5 minutes to reach 240 °C,
The extracted liquid was received into this temperature was maintained for 50 min
a trap. Once the process was over, apparatus [Marangon et al., 2008].
was disconnected and allowed to cool; volume
of oil obtained was determined and stored as Essential oils physical properties
explained in the previous section. Refractive index was determined
Factorial design using a digital refractometer (Atago, Japan).
A two-level factorial design with a The refractometer was calibrated with
confidence level of 95% was analyzed using distilled water and then dried with paper to
Minitab 16 software (Minitab Inc., State place a drop of essential oil; determination
College, PA, U.S.A.) in order to determine was carried duplicate. Due to the unique
the effects of the three variables tested compound composition of each essential
(amount of water, microwave power and oil, a significant change in the refractive
extraction time). Table I presents the index regarding the extraction method let
factors and levels tested. conclude that the extraction method affects
the composition of the essential oil. Density
Table I. Parameter values of the three factors tested. was determined using the mass volume ratio
Factor Low level (-) High level (-) by weighing 0.1 mL of essential oil.
Microwave power (W) 70 80
RESULTS
Time (min) 20 30
The complete experiments and the
Amount of water (mL) 400 500
yields of basil and epazote essential oils
obtained in each condition of the factorial
Optimization of the yields of basil and design for MAE are shown in Table II. The
epazote essential oils by MAE whole experiments were done for basil, and
In order to determine the influence for epazote, selected conditions were carried
of the factors and their levels, the yields out (those in which the highest, the lowest
obtained were analyzed and the p value and medium yields were observed for basil).
of the factors and their interactions were Higher yields (0.47 and 0.39% for basil
calculated. Through the two-level factorial and epazote, respectively) were obtained
design statistical analysis, contour plots with the combination of 70% of power, 30 min
were constructed in order to optimize the of microwave heating and 400 mL of water.
extraction conditions, that maximize the Basil essential oil yield was found not to
yield of the essential oils. be significantly different (p<0.05) with
respect to the oil obtained by SD extraction
Essential oils chemical composition (0.50±0.06%); however, epazote essential oil
Chemical composition of essential yield was found to be significantly different
oils was determined by gas chromatography (p<0.05) in comprison with the oil obtained
coupled to mass spectrometry detector (GC- by SD extraction (0.20±0.008%). On the other
MS) in a chromatograph (Agilent Technologies hand, the lowest yields (0.15 and 0.21% for
model 6850N) equipped with a triple axis basil and epazote, respectively) were obtained
mass detector (5975C). A capillary column with the combination of 70% of power, 20 min
(HP5-MS) was used for the separation of and 500 mL of water.
the components, using chromatographic Figure 2 shows a visual comparison
grade helium as carrier gas at constant flow of the higher yields of essential oil of basil
Table II. Experiments order of the factorial design and yields of basil and epazote essential oil obtained.
Microwave power Time Amount of water Yield (%)
(W) (min) (mL)
Basil Epazote
70 30 500 0.36 0.33
80 20 400 0.32 ----
70 20 500 0.15 0.21
70 20 400 0.25 ----
80 30 500 0.41 0.36
70 30 400 0.47 0.39
80 30 400 0.45 ----
80 20 500 0.15 ----
Figure 3. Contour plot of the interaction of the two significant affecting parameters on the yield of essential oil.
Table IV. Main components in essential oil of two herbs obtained by MAE and SD.
Compound
Herb
MAE SD
methyl cinnamate methyl cinnamate
linalool cadinol
Basil eucalyptol linalool
β-cubebene β-cubebene
cadinol eucalyptol
a, 4 - trimethyl -, acetate (+) -4 - Carene
(+) - 4 - Carene limonene oxide, cis
Epazote limonene oxide, cis androst - 1 - en - 3 -one, 4, 4 -dimethyl
azabicycle [2. 2. 2] octane - 3 - one a-terpinene
1 - cyclohexane - 1 - carboxaldehyde, 4 cyclohexane, 1 - methyl -3 - (1 -
-(1-methylethyl) methylethylene)
Table V. Physical properties of essential oils of two herbs obtained by MAE and SD.
Refractive index Density (kg/m3)
Method Basil Epazote Basil Epazote
MAE 1.4984±0.001a 1.478±0.00a 927±0.01a 906±0.004a
SD 1.5079±0.011a 1.478±0.00a 937±0.01a 882±0.002b
For epazote essential oil, a higher density reported slightly higher yields of essential
in the essential oil extracted by MAE was oil of oregano with MAE in respect to SD. In
observed. addition to the innate composition of the
herb, several authors [Omer, 1999; Boyle
DISCUSSION et al., 1991; Baranauskiene et al., 2003]
Even there was not control of have attributed the high or low yields of
the internal temperature, acceptable essential oils to the level of fertilization
repeatability between experiments were of the soil where the herb is planted, by
achieved. This was attributed to a small directly affecting the phenolic compounds
cavity and relative low power employed in content [Musika, 1993].
the study. Martin (2008) suggested than in High temperatures and different
small cavities the waves are dispersed in heating conditions which herbs are subjected
better way than big cavities, improving the in both methods are a determinant factor
uniformity during microwave heating. in the chemical composition of essential oil
The results of yield percentage extracted; Alitonou et al. [2012] describe
of essential oil obtained from basil and some compounds as fragile molecules and
epazote let say that in addition to provide sensitive to the thermal shocks and the
the advantages already mentioned the chemical aggressions. Owing to the different
MAE technique does not affect the final temperatures reached in each process,
yield of the oil. In 2007, Lucchesi et al., the variation of method can result in the
reported that for the extraction of Eletaria disappearance of certain compounds or in
cardamomum L. essential oil, that the a different abundance from one method to
microwave power, the amount of solvent other as shown in the chemical composition
and time of extraction significantly affected of essential oils of epazote. Under these
the yield of the essential oil. specific circumstances, although the use
Results of basil essential oil yield of MAE may offer advantages over SD, the
are similar to those reported by Ijaz et al. use of this technique can be discarded if it
[2008] in a previous study of extraction is desired to obtain a specific compound of
of essential oils from basil, in which the essential oil for a particular purpose.
yields were ranged between 0.5 and 0.8%. Despite this, in 2008, Gomez conducted
Moreover, the low yields obtained with both a study in which identified the major
methods of extraction for the essential oil components of essential oil of epazote,
of epazote may be attributed to the innate reporting that they mainly are ascaridol,
composition of the herb. However, a yield transpinocarveol, aritasone, β-pinene,
of 0.3% was reported for Alitonou et al. myrcene, phellandrene, camphor, limonene
[2012] in the extraction of essential oil of and α-terpinene, the latter two are also
Chenopodium ambrosioides L. harvested within the major compound detected in this
in different months, and by Jardim et al. study.
[2010] in the extraction of essential oil For extraction of basil essential oil,
of Brazilian Chenopodium ambrosioides the method did not affect its chemical
L. In literature, similar yields have been composition, greater number of compounds
reported in the extraction of essential oils were detected in oil obtained by MAE,
from herbs using both methods, Chemat resulting in a further advantage of the
et al. [2006] extracted essential oil from method proposed for this specific herb. The
lavender (Lavandula angustifolia Mill) presence of linalool, methyl-cinnamate and
with MAE and SD and obtained very similar β-cubebene in basil essential oil was also
results, 8.86% for the former and 8.75% for reported by Simon et al. [1999], which
the second; moreover, Beste et al. [2008] described the major components of 6 kinds
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