Current Organic Chemistry, 2011, 15, 237-247 237

The Extraction of Natural Products using Ultrasound or Microwaves

T. J. Mason1,*, F. Chemat2 and M. Vinatoru3

1
Sonochemistry Centre, Faculty of HLS, Coventry University, Coventry CV1 5FB, UK
2
UMR A 408 INRA, Université d'Avignon, Sécurité et Qualité des Produits d'Origine Végétale, 33, rue Louis Pasteur, 84029 Avignon
cedex 1, France
3
ReEnergy LLC, 6170 Research Road, Ste 202, Frisco, Texas 75034, USA

Abstract: Over the centuries mankind has benefited from the natural materials that occur in plants. In earlier times the whole plant or an
extract was used in cooking or as a medicine but nowadays the active constituents of plant extracts provide targets for the synthetic chem-
ist. In this review we will explore the advantages that accrue from the incorporation of either ultrasound or microwaves in the extraction
process. The two techniques offer different approaches in that ultrasound is generally used to improve conventional solvent extraction
whereas microwaves are known for their ability to remove constituents via heating without solvents.

Keywords: Extraction, assisted, ultrasound, microwave, solvent, without solvent.

1. GENERAL INTRODUCTION
Even before the dawn of agriculture humanity had learnt to use
herbs and plants for foods, as flavouring additives and as a medi-
cine. There is a very long history of uses for medicinal herbs all
over the world with perhaps the best known being Chinese tradi-
tional herbal medicine with written recipes dating back thousands
of years and Egyptian papyruses describing the use of medicinal
herbs.
Nowadays the main uses of herbal extracts are medicinal with
an ever-growing interest in nutritional supplements often termed
nutriceuticals. In the last century the interest for herbal medicine
declined in favour of synthetic drugs but this interest has now been
revived due to the discoveries of many new and powerful drugs that
are obtained from plants. A few of these are shown in Fig. (1) with
their structures e.g. paclitaxel 1a, extracted from yew tree and used
in cancer therapy; tamiflu, used to combat flu diseases, has as base
material shikimic acid 1b, extracted from Star Anise; quinine 1c,
extracted from the bark of the cinchona tree, used for malaria
treatment, artemisin 1d, extracted from Artemisia annua another
drug to combat malaria, etc.
Fig. (1). Chemical structures of some well known natural medicines: a)
Aspirin, acetyl salicylate, is one of the most widely used medi- Paclitaxel, b) Shikimic acid, c) Quinine, d) Artemisin.
cines and is prepared by chemical syntheses – but its precursor,
salicylic acid, is found in willow tree bark. Some natural remedies ern methods that have been developed to extract bioactive ingredi-
such as anti rheumatic ointments are also derivatives of salicylic ents are ultrasonically assisted extractions (UAE) and microwave
acid. Thus methyl salicylate which is a powerful compound used to assisted extraction (MAE). UAE is a technique that dates back in
fight rheumatic pain was known and used by Native Americans in 1950s when the first laboratory scale experiments were reported [1]
the USA and was obtained from birch tree bark. but MAE is more modern with its roots in extracting components
for analytical purposes in the 1980s [2]. In this review we will con-
In principle the plant world could provide a renewable resource
sider the methods separately since the former generally involves
of raw materials for pharmaceutical, cosmetics, food, fuel and
solvent and the latter has applications which do not involve the use
chemical industries. With current interests focussing on green and
renewable sources for these industries a new term “biorefinery” has of solvents.
appeared to cover emerging technologies based in this area. There are a few cases where a combination of ultrasound and
microwave technology have been reported to improve extractions
Over the long history of using herbs as medicines a key goal
has been to find new ways to obtain extracts enriched with active but this is a very new field of research.
constituents so that they have a more powerful action. Among mod-
2. ULTRASONICALLY ASSISTED EXTRACTION (UAE)
2.1. General Introduction to UAE
*Address correspondence to this author at the Sonochemistry Centre, Faculty of HLS, The extraction of food additives and nutraceuticals from plants
Coventry University, Coventry CV1 5FB, UK; Tel: +44 (0) 2476 888173; Fax: +44 (0)
2476 888173; E-mail: t.mason@coventry.ac.uk or seeds requires the use of an appropriate solvent and a method of

1385-2728/11 $58.00+.00 © 2011 Bentham Science Publishers Ltd.

238 Current Organic Chemistry, 2011, Vol. 15, No. 2
Fig. (2). Unit operation scheme for solvent extraction from plant sources.
ensuring that the material has sufficient contact with that solvent.
Often the plant material is chopped or crushed to increase this con-
tact area. Additional stirring is also used and prolonged contact is
often necessary to achieve high levels of extraction. In principle it
is possible to use fresh or dry biomass. The fresh biomass has the
advantage of little preparation and minimal deterioration of the
target bioactive compounds. There is however the problem that it
can contain over 70% of water which will dilute the extraction sol-
vent. The water content is also a problem with the preparation of
the raw materials because it hinders shredding and grinding. Dry
biomass, even if it is bulk herb, is easier to grind to the required
size prior to extraction. Also it is much easier to control the sol-
vent/herb ratio, offering greater reproducibility in experimental
work.
The use of ultrasound can enhance the extraction process by in-
creasing the mass transfer between the solvent and plant material.
In addition the collapse of cavitation bubbles leads to better cell
disruption via the formation of microjets due to asymmetrical bub-
ble collapse near a solid surface. This allows for improved solvent
penetration into the plant body itself and can also break down cell
walls [3]. As a consequence, employing ultrasound in the use of
plant extraction has benefits in increased mass transfer, better sol-
vent penetration, less dependence on solvent used, extraction at
lower temperatures, faster extraction rates and greater yields of
product [4, 5]. These features make sonication an attractive propo-
sition for many extractions and for scale-up it should be used in the
extraction unit itself where the plant material is in direct contact
with the solvent e.g. in the extraction of anti-oxidants from Rose-
mary [6].
2.2. Possible Operations in which UAE could be Used in Gen-
eral Extraction Processes
In a typical extraction the operation unit scheme consists in sol-
vent extraction unit that could be:
a) solvent (water or organic solvents) extraction of
plant components
b) maceration with water or alcohol-water mixture
c) boiling with water (infusion)
d) extraction with cold fat (enfleurage)
e) extraction (maceration) with hot fat, etc.
f) liquid carbon dioxide extraction (including super-
critical state)
g) extraction using refrigeration fluids
Mason et al.
Of the 7 types of extraction operations listed above sonication
can be applied to the solvent extraction process (a) and, less com-
monly, to maceration (b) and supercritical carbon dioxide extraction
(f). Although in principle ultrasound can be applied to pressurised
refrigeration fluids there is no data available to date on this. Ultra-
sound could also be of help during evaporation [7]. The unit opera-
tion scheme with the points at which ultrasound could be employed
is given in the Fig. (2).
2.3. Solvent Extraction Parameters
The extraction mechanisms are different for fresh and dry bio-
mass. In the former case the extraction is mostly ruled by diffusion,
due to the concentration gradient between the plant material and
surrounding solvent whereas in the case of dry biomass the first
step is a swelling of the dry material by solvent uptake into the
plant cells. Solvent uptake is one of the most important steps in dry
herb extraction, so much so that it is defined in the British Pharma-
copoeia [8] as swelling index (SI) and is the volume in ml of liquid
taken up by the swelling of 1 g of plant material under specified
conditions. Ultrasound speeds up this process by asymmetrical
bubbles collapse near to the plant surface which forces the solvent
into the dry material thus enhancing the swelling process. A com-
parison of classic and ultrasonic swelling indices for a range of dry
plant material is given in Fig. (3) [3].
We know that ultrasound can be used to improve extraction but
in what way could this be quantified ? A parameter that can be ap-
plied to extraction procedures is the extractive value (EV) which is
normally quoted in terms of the mass of target material (g) ex-
tracted from 100 g of starting material by a standard method. In
Table 1 the ultrasonic extractive value was chosen as being the dry
residue obtained with a half hour steeping and one hour sonication
(compared with classical 23 hours steeping and 1 hour stirring) [3].
Ultrasound is beneficial for both the swelling and extractive in-
dices. In addition the data in Table 1 shows that different solvents
give different EV’s thus before performing any experimental work
regarding herbal extraction it is always useful to test the extractive
value for several solvents or solvent mixtures.
It is important to recognise that these effects occur only when
the plant material is in the ultrasonically agitated zone of the reactor
and so a stirrer is often used in addition to an ultrasonic source.
Such stirring will have the additional advantage that it will keep all
of the particles in suspension and avoid the accumulation of bio-
mass on the bottom of the reactor.
The Extraction of Natural Products Current Organic Chemistry, 2011, Vol. 15, No. 2 239

Fig. (3). The effect of ultrasound on swelling index for a range of dry plant material.

Table 1. Comparison of Classic (Silent) and Ultrasonic Extractive Values for Some Plant Materials

Plant Method Eth Eth/W W Gly/W Ether

Classic 10.2 7.4 8.2 13.4 12.2

Fennel seeds 1/2 h UAE 13.7 7.3 11.0 13.4 16.0

1 h UAE 14.3 7.5 15.6 15.2 19.3

Classic 20.4 27.0 24.0 22.5 4.5

Hops strobiles 1/2 h UAE 22.8 31.0 28.3 28.0 6.3

1 h UAE 27.0 32.0 29.5 31.0 7.2

Classic 16.0 20.0 30.0 22.5 14.8

Pot marigold 1/2 h UAE 16.5 22.0 30.5 27.8 15.6

1 h UAE 18.0 23.0 31.4 28.0 16.8

Classic 16.2 16.3 21.4 -

Peganum seeds 1/2 h UAE 17.3 17.0 22.0 -

1 h UAE 19.0 18.6 22.0 -

Classic 8.5 21.3 26.4 24.6 3.2

Mint leaves 1/2 h UAE 9.3 26.3 26.5 25.2 3.6

1 h UAE 9.7 26.8 26.8 26.7 4.2

Classic 8.6 21.1 21.3 32.2 -

Lime flowers 1/2 h UAE 8.7 21.6 24.4 33.5 -

1 h UAE 10.0 25.0 25.1 34.8 -

Classic 14.2 7.6 7.6 9.9 -

Elecampane root 1/2 h UAE 17.5 6.7 9.2 10.6 -

1 h UAE 17.9 6.5 9.2 14.3 -

Eth = 94 v/v Ethanol/water; Eth/W = 70 v/v ethanol/water; W = water; Gly/W = 3.5 v/v glycerol/water; Ether = diethyl ether.

2.4. The Mechanism of UAE
There are several properties of ultrasound that can increase the
efficiency of solvent extraction.
2.4.1. Improved Diffusion
When a solvent is in contact with the plant material it will sur-
round it and begin the slow process of penetration leading to swel-
ling. In the majority of cases the solvent is ethyl alcohol either neat
or as an aqueous mixture both of which will develop hydrogen
bonding with the OH groups of cellulosic main structure of the
material. This superficial layer of solvent will hinder the extraction
efficiency by obstructing the diffusion process that is itself gov-
erned by the concentration gradient. This surrounding layer is quite
highly loaded with the extracted compounds from the plant and
because it is adherent it will stay unperturbed and diminish the ex-
traction rate. In classical extraction the most used technique for
disturbing the layer is by stirring (particularly if the extraction is to
be performed at room temperature). An alternative to stirring is to
raise the solvent temperature, provided that the target extract is not
thermally sensitive.
240 Current Organic Chemistry, 2011, Vol. 15, No. 2
Using ultrasound the superficial layer is continuously removed
by the high-speed jets formed during asymmetrical bubble’s col-
lapse, letting fresh (or less loaded) solvent enter the surrounding
layer thus enhancing the diffusion process.
2.4.2. Improved Mass Transfer
In addition to disrupting the superficial solvent layer by ultra-
sound the intense mechanical agitation effect also plays an impor-
tant role in providing better mass transfer. Cavitation bubble col-
lapse generates sufficient energy to cause collisions between sus-
pended plant particles as in the case of classical extraction by stir-
ring.
2.4.3. Breakdown of Plant Cells
Acoustic cavitation provides enough energy to break down the
plant material releasing the cell content. In addition the mechanical
action will reduce particle size allowing much more plant surface to
be in contact with the extraction solvent. However the latter can
result in the formation of a suspension of very fine plant material
that is very difficult to filter. Thus it is necessary to find a balance
between improving the extraction efficiency whilst keeping subse-
quent post-processing steps viable and economic. This is always
necessary when considering UAE on an industrial scale.
2.4.4. Improved Solvent Penetration
Sonication can produce a better penetration of solvent into the
plant cells through the jet generated by bubble collapse. The jet can
enlarge the cell pores and effectively act as a micro-pump, pushing
solvent into the cell dissolving the components and transporting
them outside. This contributes to the intensification of mass transfer
and provides many advantages for extraction.
2.4.5. Capillary Effects of Ultrasound (Sonocapillary Effect)
The sonocapillary effect is an anomalous rise of a liquid in a
capillary tube under the action of ultrasound and was discovered in
the 1960’s. Although it can be easily demonstrated in the laboratory
it has not been widely investigated [9]. Since some components
such as essential oils are in the capillary system of a plant material
it would be expected that ultrasound could help expelling them by
sonocapillary effect. It is possible that some electrical phenomena
accompanying the sonocapillary effect might also have an influ-
ence. Known as the I and U-effect they were described by Ueda in
1951 [10, 11]. The authors showed that when ultrasound was ap-
plied to a capillary glass tube containing an electrolytic an alternat-
ing electrical field was developed solution at both ends of a capil-
lary. This phenomenon could improve extraction of polar or ionic
compounds, somewhat like electrophoresis. There is no reference to
date regarding either aspect of the sonocapillary effect in ultrasonic
assisted plant extraction but we believe that both will be present.
2.5. Examples of UAE
There have been a large number of papers published dealing
with UAE and the subject was reviewed thoroughly in 1999 [4] and
subsequently in 2001 [5]. However a few specific examples will
help to show the range of possibilities using this technique.
2.5.1. Laboratory Extractions
Polymeric compounds. Corn cob xylan and corn bran hemicel-
luloses can be successfully extracted by aid of ultrasounds, as re-
ported by Hromadkova et al. [12, 13]. The same group have ex-
tracted polysaccharides from valerian roots remaining after tincture
Mason et al.
preparation [14]. The authors noted that sonication causes de-
polymerization of the solubilised polysaccharides yielding aqueous
ethanol soluble fragments. Lignin could be extracted under alkaline
conditions using ultrasound without significant changes in lignin
composition and structure [15]. The use of ultrasound-assisted ex-
traction technique decreases the total time of treatment for cellulose
isolation and the obtained purity of cellulose was very high [16].
Oils. Several papers relate the use of ultrasound in vegetable oil
extraction. Thus, in olive oil extraction, the high power ultrasonic
pretreatment of olive paste has shown a positive effect on the
churning step [17]. Tobacco seeds, a by-product of tobacco leaf
production, are a source of vegetable oil and ultrasonically assisted
hexane extraction has been investigated. Although soxhlet extrac-
tion was more efficient overall the advantage of UAE was a rela-
tively high oil yield at 25°C in a shorter time [18]. Extraction of
soybean oil using, isopropanol and 3:2 hexane-isopropanol mixture
was performed with ultrasound and was shown to improve effi-
ciency and reduce processing time, especially when mixed solvents
were employed [19].
Bleaching is the most critical step in vegetable oil refining and
is normally accomplished by treating the oil with acid activated
clays. The main advantage of sonication in this technique is that it
decreases the bleaching time required, and this avoids the harmful
side-effects of bleaching with acid-activated earths by minimizing
the time and the temperature required [20].
It has also been reported that presonication could bring benefits
for some extraction processes. Thus, aqueous enzymatic oil extrac-
tion from almond and apricot seeds gives better yields when the
extraction mixture was pre-irradiated with ultrasound for 2 minutes
[21].
2.5.2. UAE in Supercritical CO2
Until recently the use of ultrasound in supercritical fluids ex-
traction was not considered due to difficulties envisaged in the in-
sertion of an ultrasonic transducer into high pressure supercritical
CO2 extraction cell. Riera et al. has succeeded in doing this for the
extraction of almond oil using a probe operating at 20 kHz and 100
w [22]. An enhancement of the extraction yield with 20 to 30% was
obtained in this way. Balachandran et al. used a much powerful
probe system, 20 kHz and 500 watts, to extract the pungent com-
pounds from ginger [23]. They observed a 30% improvement of
extraction which was attributed to disruption of the cell structure
and an increase in the accessibility of the solvent to the internal
particle structure, which enhance the intra-particle diffusivity. Ai-
jun Hu et al. used similar experimental setup to extract oil and coix-
enolide (a 2,3-butanediol fatty acids ester) from adlay seeds and
reported a 14% increase of the extraction yield [24].
2.5.3. Miscellaneous
Sonication has been employed for the extraction of antioxidants
from the herb rosemary [25]. This increased the extraction effi-
ciency of carnosic acid from Rosmarinus officinalis. The authors
showed that sonication is more effective compared with thermal
methods with the majority of the target compounds extracted within
15 minutes. One important observation was that sonication also
appears to reduce dependence on the extraction solvent used. Thus
yields were greatly enhanced when ethanol was employed and
ethanol is a poor solvent when used under classical conditions.
Date syrup production can be accelerated with ultrasound under
ultrasonic irradiation [26]. Anthraquinones were extracted from
Morinda citrifolia [27] and xyloglucan from apple pomace [28]
The Extraction of Natural Products Current Organic Chemistry, 2011, Vol. 15, No. 2 241

Table 2. Ultrasonically Assisted Extraction of Different Plant Materials

Targeted Ultrasonic Device

Entry Herb Extracted Characteristics Observation Reference
Compound Used

Ilex paraguariensis Ultrasonic cleaning Ultrasonic methods better

1 All 40 kHz, 0.27 W/cm2 [30]
leaves bath than maceration

Honey from Robinia

Ultrasonic cleaning Solvent: pentane-ether
2 pseudoacacia & Cas- Volatile compounds 35 kHz [31]
bath (1:2)
tanea sativa

3 Red raspberries Anthocyanins Ultrasonic horn 22 kHz, 650 W 1.5 M HCl-95% ethanol [32]

Chloroform
Methanol
22.4 kHz, 240 W, pulse Acetonitrile
4 Vanilla pods Vanillin Ultrasonic horn [33]
mode 5s on 5s off Ethanol
Acetone
Hexane
Ultrasonic cleaning Water/ethanol 50/50%
5 Cocos nucifera Phenolic compounds 25 kHz, 150 W [34]
bath (v/v) pH=6.5 (HCl)

Methanol
Ultrasonic cleaning 20, 60 and 100 kHz, variable
6 Citrus reticulata peel Hesperidin (flavonoid) Ethanol [35]
bath power
Isopropanol
Epimedin A, B, C and Ultrasonic cleaning
7 Herba Epimedii 28 kHz, 500 W Ethanol 0-90 % (v/v) [36]
icariin bath

8 Rheum palmatum L. Anthraquinones Ultrasonic humidifier 1.7 MHz, 35 W 80% ethanol [37]
Ultrasonic cleaning 35 kHz, 600 W
bath, lab study
9 Capsicum frutescens capsaicinoids 20 L Ultrasonic stirred Ethanol 95% (v/v) [38]
tank with transducers
bonded to walls 26 and 70 kHz, 1.08 kW
Phenolics-rich hetero- 0.5, 2 and 5% NaOH
10 Wheat bran Ultrasonic horn 20 kHz, 100 W [39]
cylans solution

Ultrasonic cleaning
11 Citrus peel Phenolics 60 kHz 80% methanol [40]
bath

Dual or triple frequency

combinations:
Peanuts (Arachis hy- Isoflavones and Trans- Ultrasonic cleaning 25 and 40 kHz;
12 80% ethanol [41]
pogaea) resveratrol bath 25 and 80 kHz;
40 and 80 kHz and 25, 40
and 80 kHz

13 Carvone-rich plants Flavour compounds Ultrasonic probe 20 kHz, 200 W 70% ethanol (v/v) [42]

Bioactive principles Quillaja Saponaria

14 Ultrasonic probe 20 kHz, 30-70 W Water [43]
(saponins) Molina
Hexane-isopropanol-
15 Phospholipids Palm-pressed fiber Ultrasonic probe 24 kHz, 300 W [44]
water

Water:ethanol 1:1, 2:3

16 Dye component Beetroot Ultrasonic probe 20 kHz, 400 W [45]
and 3:2

Methanol
Ultrasonic cleaning
17 Salvianolic acid B Salvia miltiorrhiza 28, 45 and 100 kHz, 100 W Ethanol [46]
bath
n-butanol

Hydrodistillation,
Lavandula angustifolea Superctical extraction and
18 Flavour compounds Ultrasonic probe 20 kHz, 200 W [47]
L. ultrasonic
compared

with better results than classical methods. Application of ultrasound
to grape mash treatment for juice extraction enhances extraction,
shortens the treatment time and improves the juice quality [29].
A summary of recent papers dealing with UAE is given in
Table 2.
2.6. Industrial UAE Extraction Technology
One of the main problems when any new laboratory technique
appears in the literature is how it could be scaled up for pilot or
industrial applications. In a recent paper Paniwnyk et al. studied the
anti-oxidants extraction from Rosmarinus officinalis using ultra-
242 Current Organic Chemistry, 2011, Vol. 15, No. 2
sound at a laboratory scale as well as pilot scale [6]. Thus, they
used as larger volume reactor a 125 L ultrasonic cleaning bath
showing that even at this scale the extraction time was shorter and a
greater yield was obtained compared with a classical thermal proc-
ess.
The saponins in ginseng were extracted from ginseng roots and
in this process ultrasonic extraction was not only more efficient but
also convenient for the recovery and purification of the active in-
gredients [48]. One type of extraction, to form a tincture, is cer-
tainly one that can be improved using ultrasound and this has been
adopted by industry [5]. An industrial ultrasonic reactor was de-
signed and built in Romania for tinctures preparation from various
herbs (Fig. 4) [49]. Using this reactor the extraction time could be
shortened from 28 days to 10 hours with similar or better outputs.
Fig. (4). Industrial ultrasonic reactor for the extraction of herbs (1000 L).
Fig. (5). Flow loop type industrial ultrasonic reactor.
A different approach to the design of an industrial reactor was
made in South Africa, Fig. (5) [50]. This is a circulating loop type
Mason et al.
reactor. The ultrasonic transducers were mounted in separate cylin-
ders and connected to the main tank (2000 L). The suspension of
herbs in solvent is pumped into the external ultrasonic reactors until
the desired concentration of bioactive components was reached.
Sage and valerian extracts were industrially obtained in Slovak
Republic and compared with classical tinctures of same herbs [51].
The authors noticed that greater improvement for sage compared
with valerian and also that continuous ultrasound applied continu-
ously throughout the extraction brought about better results. Such
extended sonication was disregarded for economic reasons and a 30
minute burst of sonication was used instead.
3. MICROWAVE ASSISTED EXTRACTION (MAE)
3.1. General Introduction to MAE
Microwave heating (2.45 GHz) occurs as the result of the dis-
sipation of electromagnetic waves in the irradiated medium. The
dissipated power in a medium depends on the dielectric properties
and the local time average electric field strength. So, there is a fun-
damental difference between microwave and conventional extrac-
tion (Fig. 6). In conventional solvent extraction, mass transfer oc-
curs from the inside to the outside while heat transfer occurs from
the outside to the inside. In contrast for microwave solvent extrac-
tion, these transport phenomena are both in the same direction from
the inside of the extracted material to the bulk solvent. The accel-
eration of extraction rates under microwaves could be due to a syn-
ergy combination of the two transfer phenomena mass and heat
acting in the same direction. In MAE, heat is dissipated throughout
the whole volume inside the irradiated medium, while in conven-
tional extraction, heat is transferred from the heating medium
through the outer part of the sample to the interior. This results in
an important difference between conventional and microwave heat-
ing. In the former heat transfer depends on thermal conductivity and
on the temperature difference across the sample and the exterior
and in the case of fluids, on convection currents. As a result, the
temperature increase is often rather slow. In contrast to this, in mi-
crowave heating, due to the heating effect on the whole volume a
much faster temperature increases can be obtained, depending on
the microwave power and the dielectric loss factor of the material
being irradiated.
Fig. (6). Illustration of difference between microwave and conventional
extraction.
Ganzler described the use of microwave energy to assist the iso-
lation of chemicals from bulk materials in the chemical laboratory
for the first time in 1986 [52]. This report dealt with the extraction
of pollutants from sewage sludge but since then, numerous labora-
tories have studied the analytical possibilities of microwaves as a
The Extraction of Natural Products Current Organic Chemistry, 2011, Vol. 15, No. 2 243

non-classical energy source. Today, over 1000 articles have been temperature, power and/or pressure so MAE reactors can be
published on the subject of microwave extraction. It is likely that equipped with an IR and/or fiber optic thermometer, pressure gauge
the acceleration of extraction rates under microwave irradiation are and a camera to follow the extraction and software to regulate the
due to a combination of the two transfer phenomena mass and heat microwave power [57-60].
both acting in the same direction which are conventionally in oppo- In order to facilitate industrial trials, Archimex has developed
site directions during conventional extraction [53, 54]. reactors from 50 to 200L (Figs. 8 and 9). Continuous systems are
coupled to microwave in order to enhance the quality and quantity
3.2. MAE Reactor Designs of extraction yield and to reduce processing time [61, 62].
With the advances that have been made in microwave technol-
ogy over recent years a wide range of configurations have been
developed for MAE extractions with the choice depending on the
type of raw material and targeted extract (analyte).
In general there are two kinds of microwave ovens to be found
in laboratories differing by their cavity: single-modes (also called
mono-modes or focused modes) and multi-modes (Fig. 7). In a
single-mode cavity only one type of frequency is generated allow-
ing only one mode of resonance to be excited. In such a case, the
sample must be placed in a specific position in order to receive a
maximum of microwave energy. It ensures a direct and efficient
application of high density microwave energy on the sample matrix,
inducing a rapid heating of the medium with a fast extraction of the
analyte. However, mono-mode systems are quite limited in term of
volume and quantity of sample that can be extracted. On the other
hand multi-mode ovens are larger and allow several modes of reso-
nance so that a number of different of incident waves can be ap-
plied on the sample. This kind of oven can be used to extract much
larger quantities of raw material employing several different con-
figurations of extraction vessel. A turntable is often used to allow
an even distribution of the incident waves in the oven and for such a
system scale-up is more convenient [55, 56].
Fig. (8). Continuous microwave solvent extraction (www.archimex.com).

Fig. (9). Vacuum microwave hydrodistillation (www.archimex.com).

Fig. (7). Focused and multi-mode cavity microwave ovens.
Special laboratory microwave extraction reactors (from 0.1 to 1
L) has been developed by Milestone (www.milestonesrl.com, Italy).
The microwave intensity is about 1 W/g at a frequency of 2.45
GHz. In such systems it is best to regulate and maintain constant
3.3. MAE Techniques
Since the publication of Ganzler in 1986 [52] advances in mi-
crowave extraction have resulted in a number of techniques such as
microwave-assisted solvent extraction (MASE) [63], compressed
244 Current Organic Chemistry, 2011, Vol. 15, No. 2 Mason et al.

Table 3. Comparison of Microwave Assisted Extraction Techniques for Natural Products

Extraction techniques

MASE CAMD VMHD SFME MHG

Microwave Assisted Compressed Air Microwave Vacuum Microwave Solvent Free Micro- Microwave Hydrodiffu-
Name
solvent Extraction Distillation HydroDistillation wave Extraction sion and Gravity

Sample is immersed in a Sample is irradiated by microwave Sample is submitted to Sample without any Sample without any solvent
non microwave-absorbing under an air flow in order to take microwave combined with solvent is submitted to is submitted to microwaves
Brief description
solvent of the volatile oil. sequential vacuum microwaves and separation is done by
gravity

Extraction time 3-30 min 5 min 3-30 kg/h 10-60 min 5-15 min.

Sample size 1-10 g 30-40 g 0.1-1 kg 0.1-1kg

Solvent usage 10-40 ml Air pump No solvent No solvent No solvent

Investment Moderate Low High Low Low

 Fast and multiple extrac-  Fast and easily to realize  Fast  Fast, green economi-  Fast, green and economi-
tion  Head note accentuated cal cal
Advantages
 Low solvent volumes  Volatile oil highly 
odoriferous  highly odoriferous

Waiting to
Clean-up
Difficult and expensive to

Drawbacks
cool down step needed implement

References 62 64 61 59 58

air microwave distillation (CAMD) [64], vacuum microwave hy-
drodistillation (VMHD) [61], solvent free microwave extraction
(SFME) [60], and microwave hydro-diffusion and gravity (MHG)
[58]. Table 3 summarizes the most common microwave extraction
techniques for plant matrices and presents their advantages and
drawbacks. Over the years procedures based on microwave extrac-
tion have replaced some of the conventional processes and other
thermal extraction techniques that have been used for decades in
chemical, pharmaceutical, food, and cosmetic laboratories.
MASE uses microwave energy to heat a liquid organic solvent
in contact with a sample and was first used in the extraction of sev-
eral compounds from environmental samples such as soil or pol-
luted water. MASE has also been applied to plant material in order
to extract aromatic compounds. The technique was patented in 1990
as Microwave Assisted Process (MAP) [62]. Typically, plant mate-
rial is immersed in a non-absorbing microwave solvent such as
hexane and irradiated by microwave energy. When the oil glands of
the plant are subjected to severe thermal stresses and localized high
pressures, as in the case of microwave heating, the pressure build-
up within the glands exceeds their capacity for expansion, and
causes their rupture more rapidly than in conventional extraction.
Volatile oil dissolves in the organic solvent before being separated
by liquid-liquid extraction. Aromatic compounds from different
types of plants have been extracted by MASE from wood, roots,
leaves or seeds. In all cases, yields and composition of microwave
extracts are comparable to those obtained by a classical solvent
extraction such as Soxhlet extraction but have been achieved with
reduced extraction time [65].
One of the first methods using microwave assisted extraction of
essential oil was presented in 1989 by Craveiro [64]. The essential
oil of Lippia sidoides was extracted using only microwave energy
and compressed air. Inspired by classical steam distillation, the
CAMD technique used compressed air instead of vapor to extract
the volatile oil. Typically, plant material is placed in a reactor inside
the microwave cavity and heated whilst at the same time a com-
pressor, located outside the cavity, forces compressed air into the
reactor. Volatile oil and vapor are then driven to the recovery flask
outside the cavity. In 5 minutes CAMD provides an essential oil
which is essentially identical to that produced by the conventional
hydro-distillation method.
VMHD was elaborated and patented by Archimex in 1994 [61].
This technique is based on selective heating by microwaves com-
bined with application of sequential vacuum. The plant material is
placed in a microwave cavity with water to refresh the dry material.
The plant material is afterwards exposed to microwave radiation to
free the natural extract. Reducing the pressure to between 100 and
200 mbar allowed the evaporation of the azeotropic water-volatile
oil mixture from the biological matrix. The procedure is repeated in
a stepwise fashion in order to extract all the volatile oil from the
plant. Up to 30 kilograms per hour of material can be treated.
SFME is a recent method of extraction patented by Chemat et
al. in 2004 [59, 60] specifically aimed to obtain essential oil from
plant material. Based on a relatively simple principle, SFME in-
volves placing vegetable material in a microwave reactor without
addition of any solvent or water. SFME is a combination of micro-
wave heating and distillation, and is performed at atmospheric pres-
sure. In terms of quality and quantity, SFME appears to be more
competitive and economic method when compared with classical
methods such as hydro or steam distillation [66, 67]. SFME has
been used to obtain essential oils from aromatic herbs (basil, mint,
and thyme) [68] and spices (ajowan, cumin, and star anise) [69].
Microwave Hydrodiffusion and Gravity (MHG) is a new and
green technique for the extraction of food ingredients patented by
Chemat et al. [58] in 2008. This green extraction technique is an
original “upside down” microwave alembic combining microwave
heating and earth gravity at atmospheric pressure. MHG was con-
ceived for laboratory and industrial scale applications for the ex-
traction of food ingredients from different kind of fruits, vegetables
The Extraction of Natural Products
and aromatic plants. This method involves placing plant material in
a microwave reactor, without adding any solvent or water. The
internal heating of the in situ water within the plant material dis-
tends the plant cells and leads to the rupture of glands and oleifer-
ous receptacles. The heating action of microwaves thus frees essen-
tial oil and in situ water which are transferred from the inside to the
outside of the plant material. This physical phenomenon, known as
hydrodiffusion, allows the extract (water and essential oil), diffused
outside the plant material, to drop by earth gravity out of the mi-
crowave reactor and fall through the perforated Pyrex disc. A cool-
ing system outside the microwave oven cooled the extract continu-
ously. Water and essential oil are collected and separated in a vessel
traditionally called the “Florentine flask”. The essential oil, floats at
the top while water goes to the bottom and can be easily separated.
It is important to note that this green method allows to extract es-
sential oils without distillation and evaporation which are the most
energy consuming processes between the unit operations. MHG has
been used to obtain essential oils from aromatic herbs (mint, rose-
mary) [70, 71] and citrus fruits [72].
3.4. MAE Applications
When using microwave assisted solvent extraction there are two
approaches:
• Use a microwave-absorbing extraction solvent with a
high dielectric constant. In this technique, the sample and
solvent are placed together in a closed vessel similar to
those used for microwave digestions. Microwave radia-
tion heats the solvent to a temperature higher than its
boiling point, and the hot solvent provides a rapid extrac-
tion of analytes under moderate pressure (1-50 bars). This
approach has been successful for extracting polymer addi-
tives, vitamins in food, and priority pollutants such as
poly nuclear aromatic hydrocarbons, pesticides, and poly-
chlorinated biphenyls (PCBs) from soils and sediments
[73].
• Use of a non microwave-absorbing extraction solvent
with a low dielectric constant. Here the sample and sol-
vent can be placed in an open or closed vessel. The sol-
vent does not become hot because it absorbs very little
microwave radiation. The sample, however, which usu-
ally contains water or other compounds possessing a high
dielectric constant, absorbs the microwave radiation and
releases the heated analytes into the surrounding cool liq-
uid, which is selected according to its solubility character-
istics. This approach is gentler. Generally, it is performed
under atmospheric or low- pressure conditions and can be
used with heat-sensitive or thermally labile analytes. Ex-
amples of using this approach include the extraction of
antioxidants or oils compounds from parsley, peppermint,
cedar oil, sulfur-containing garlic components, perfumery
and flavoring volatiles from flowers, lipids from fish and
organochloro-pesticides from sediment sample.
Hemwimon [74] has made a comparison of the microwave-
assisted extraction (MAE) of antioxidative anthraquinones from the
roots of Morinda citrifolia and extraction with other conventional
techniques (maceration and Soxhlet) and ultrasound-assisted extrac-
tion (UAE). The efficiency of extraction using MAE [720W,
15min, 60°C, 10ml EtOH:H2O (80:20)] was found to be higher than
maceration (3 days, 25°C, 10ml EtOH), UAE (15.7W, 60min,
60°C, 10ml EtOH) and was also comparable with that of Soxhlet
Current Organic Chemistry, 2011, Vol. 15, No. 2 245
(4h, boiling point, 200ml EtOH). The main reason behind the
higher anthraquinones recovery with MAE was the dipole rotation
of the polar solvent in the microwave field. The extract from MAE
had higher antioxidant activity than those of UAE and maceration.
The exposure of the maceration extract to unfavourable conditions
like light and oxygen resulted in its lower activity due to long ex-
traction time.
Young [75] developed a novel MAE technique for the isolation
of ergosterol in Alternaria alternaria hyphye and spores, mush-
rooms, filtered air, artificially contaminated maize, naturally con-
taminated grain dust, and soil. Milligram-sized samples were irradi-
ated in a conventional microwave oven for 35s in the presence of
methanol and aqueous NaOH and resulted in simultaneous extrac-
tion and saponification for ergosterol. Total eregoserol was deter-
mined by reversed phase HPLC with UV detection at 282nm and
confirmed by GC-MS. Results from a variety of fungal samples
showed MAE-derived ergosterol values to be comparable with
those obtained by classical solvent extraction and significantly
better than those obtained by supercritical fluid extraction (SFE). It
was concluded that MAE procedure is simple, rapid, reliable, and
economical with respect to amount of reagents required, especially
when compared with classical solvent and SFE.
Kovacs et al. [76] have reported a microwave-assisted solvent
extraction technique for the extraction of free amino acid from food
(salami, cheese and vegetables). The method gave better yield and
reduced time required for complete sample preparation by 66%.
They also confirmed that 10% more of the amino acid was ex-
tracted from vegetables and animal samples when microwave en-
ergy was applied during the extraction of amino acid using 7%
perchloric acid as a reagent for extraction. The time necessary for
sample preparation was also reduced.
Pedro et al. [77] extracted fat from the subcutaneous tissue of
Iberian pigs by both classical solvent (2:1 chloroform-methanol for
24 h at ambient temperature) and with the use of a microwave oven
(5 min at 700 W and 2450 MHz). No significant differences was
observed in fatty acids, suggesting that the fat obtained by both
techniques was the same and that the extraction of fatty acids by
microwaves is suitable for quality classification of Iberian pig car-
casses.
Paré and Belanger [62] have used MASE for extraction of es-
sential oils from peppermint leaves. The leaves were immersed in
hexane and exposed to microwave for 30-60s in order to extract its
essential oil contents, the extracts were analysed by GC-FID and
the leaves by SEM. The efficiency of the process (levels of men-
thol, menthone, pinene and humulene) was greater for samples
treated for 50s vs those treated for 30s. Overall yields of essential
oils were also increased.
Lucchesi et al. [68] have extracted essential oils by SFME from
three aromatic herbs: basil, garden mint and thyme. With this tech-
nique the isolation and concentration of volatile compounds were
performed in a single step, without adding any solvent or water.
Essential oils extracted in this way were richer as compared to con-
ventional method in terms of amount of oxygenated compounds;
eugenol (43.2%) in basil, carvone (64.9%) in mint and thymol
(51%) in thyme. The higher abundance of oxygenated compounds
in essential oil obtained through microwave extraction is related to
the rapid heating of polar substances and to the smaller amount of
water used, which prevented the decomposition of principal oxy-
genated constituents by thermal and hydrolytic reactions. Addition-
ally the SFME method also offers a reduced environmental burden
as it releases less CO2 into the atmosphere (200g CO2 per gram of
246 Current Organic Chemistry, 2011, Vol. 15, No. 2
essential oil compared to traditional method 3600g CO2 per gram of
essential oil).
4. COMBINED UAE AND MAE
There are a few references to the combination of ultrasound and
microwave technologies in extraction. Lianfu and Zelong [78] have
described the extraction of lycopene (food colour) from tomatoes
with combined innovative techniques ultrasound and microwave
assisted extraction (UMAE) in comparison to ultrasound assisted
extraction (UAE). The results obtained with UAE did not increase
the lycopene yield (89.4%) along with enhancement of extraction
efficiency in shorter time. The reason behind this was production of
hydroxyl radicals by acoustic cavitation of ultrasound in extracts,
due to the presence of small amount of water in extract, resulted in
decomposition of lycopene. But the yield (97.4%) was increased
when extraction was performed with UMAE, with the assistances
of acoustic cavitation and fast heating of microwaves, in shorter
time and with less solvent consumption.
Cravotto et al. have combined ultrasound with microwaves to
bring about better yields when soybean-germ oil is extracted [79].
Compared with conventional methods much higher yields were
achieved with closed-vessel microwave irradiation at 120°C and
simultaneous US/MW irradiation. This paper is pointing to the
emerging technique of combined synchronous irradiation with ul-
trasound and microwaves as an experimental arrangement to per-
form extraction of useful components from herbs.
5. CONCLUSIONS
The quest for new chemical compounds from natural resources
both as food additives and for use in medicine continues to be an
active field. Within this there is the requirement to extract, analyse
and separate components more rapidly than by conventional tech-
niques. Two of the tried and tested methods available for this are
ultrasound assisted extraction (UAE) and microwave assisted ex-
traction (MAE). The former is older and is generally regarded as a
method of accelerating solvent extraction whilst the latter is a rela-
tively new technology which has special applications for the isola-
tion of volatile plant components without the need for solvent. For
analytical purposes both are very successful and in some cases have
been used to improve the isolation of target materials. For large
scale extraction UAE is a proven technology and the scale up of
MAE is in the development stage.
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Accepted: 03 December, 2009