Chapter 2

Chapter 2

Fundamentals of Microwave Extraction
Priscilla C. Veggi, Julian Martinez, and M. Angela A. Meireles
2.1 Basic Principles
2.1.1 Mechanism of Microwave Extraction
The fundamentals of the microwave extraction (MAE) process are different from
those of conventional methods (solid–liquid or simply extraction) because the
extraction occurs as the result of changes in the cell structure caused by electromag-
netic waves.
In MAE, the process acceleration and high extraction yield may be the result of
a synergistic combination of two transport phenomena: heat and mass gradients
working in the same direction [1]. On the other hand, in conventional extractions the
mass transfer occurs from inside to the outside, although the heat transfer occurs
from the outside to the inside of the substrate (Fig. 2.1). In addition, although
in conventional extraction the heat is transferred from the heating medium to the
interior of the sample, in MAE the heat is dissipated volumetrically inside the
irradiated medium.
During the extraction process, the rate of recovery of the extract is not a linear
function of time: the concentration of solute inside the solid varies, leading to a
nonstationary or unsteady condition. A series of phenomenological steps must
occur during the period of interaction between the solid-containing particle and
the solvent effectuating the separation, including (1) penetration of the solvent
into the solid matrix; (2) solubilization and/or breakdown of components; (3)
transport of the solute out of the solid matrix; (4) migration of the extracted solute
from the external surface of the solid into the bulk solution; (5) movement of the
P.C. Veggi (*) • J. Martinez • M.A.A. Meireles

LASEFI/DEA/FEA (School of Food Eng.)/UNICAMP (University of Campinas),
R. Monteiro Lobato, 80, Campinas, SP 13083-862, Brazil
e-mail: [email protected]; [email protected]; [email protected]
F. Chemat and G. Cravotto (eds.), Microwave-assisted Extraction for Bioactive 15

Compounds: Theory and Practice, Food Engineering Series 4,
DOI 10.1007/978-1-4614-4830-3_2, © Springer Science+Business Media New York 2013
16 P.C. Veggi et al.
Fig. 2.1 Basic heat and mass transfer mechanisms in microwave and conventional extraction of
natural products. (Adapted from Périno-Issartier et al. [2])
extract with respect to the solid; and (6) separation and discharge of the extract
and solid [3].
Therefore, the solvent penetrates into the solid matrix by diffusion (effective),
and the solute is dissolved until reaching a concentration limited by the characteristics
of the solid. The solution containing the solute diffuses to the surface by effective
diffusion. Finally, by natural or forced convection, the solution is transferred from
the surface to the bulk solution (Fig. 2.2).
The extraction process takes place in three different steps: an equilibrium phase
where the phenomena of solubilization and partition intervene, in which the sub-
strate is removed from the outer surface of the particle at an approximately constant
velocity. Then, this stage is followed by an intermediary transition phase to
diffusion. The resistance to mass transfer begins to appear in the solid–liquid
interface; in this period the mass transfer by convection and diffusion prevails. In the
last phase, the solute must overcome the interactions that bind it to the matrix and
diffuse into the extracting solvent. The extraction rate in this period is low, character-
ized by the removal of the extract through the diffusion mechanism. This point is
an irreversible step of the extraction process; it is often regarded as the limiting
step of the process [5].
Many forces, such as the physicochemical interactions and relationships, can be
exposed during the extraction (dispersion forces, interstitial diffusion, driving
forces, and chemical interactions), and the persistence and strength of these
phenomena may be closely tied to the properties of the solvent (solubilization
power, solubility in water, purity, polarity, etc.) [6].
2 Fundamentals of Microwave Extraction 17
Fig. 2.2 Schematic representation of yield versus time in extraction processes. (Adapted from
Raynie [4])
2.1.2 Mechanism of Microwave Heating
In the microwave heating process, energy transfer occurs by two mechanisms:

dipole rotation and ionic conduction through reversals of dipoles and displacement
of charged ions present in the solute and the solvent [7, 8]. In many applications
these two mechanisms occur simultaneously. Ionic conduction is the electrophoretic
migration of ions when an electromagnetic field is applied, and the resistance of the
solution to this flow of ions results in friction that heats the solution. Dipole rotation
means rearrangement of dipoles with the applied field [8].
Energy transfer is the main characteristic of microwave heating. Traditionally, in
heat transfer of the conventional process, the energy is transferred to the material by
convection, conduction, and radiation phenomena through the external material sur-
face in the presence of thermal gradients. In contrast, in MAE, the microwave energy
is delivered directly to materials through molecular interactions with the electro-
magnetic field via conversions of electromagnetic energy into thermal energy [9].
The most important properties involved in microwave processing of a dielectric
are the complex relative permittivity ( ε ) and the loss tangent (tan d) [10, 11]:
ε = ε ′ − jε ′′ (2.1)
ε ′′
tan δ = (2.2)
ε′
where
j = −1 (2.3)
Table 2.1 Physical constants and dissipation factors for solvents usually used in microwave-assisted
extraction (MAE) [14, 15]
Dieletric constant,a Dissipator factor Boiling Viscosity,c
Solvent ε ′ tan d (×10 −4
) point, b
(°C) (cP)
Acetone 20.7 5,555 56 0.30
Acetronitrile 37.5 82
Ethanol 24.3 2,500 78 0.69
Hexane 1.89 69 0.30
Methanol 32.6 6,400 65 0.54
2-Propanol 19.9 6,700 82 0.30
Water 78.3 1,570 100 0.89
Ethyl acetate 6.02 5,316 77 0.43
Hexane–acetone (1:1) 52
a
Determined at 20°C
b
Determined at 101.4 kPa
c
Determined at 25°C
The material complex permittivity is related to the ability of the material to interact
with electromagnetic energy, whereas ε ′ is the real part, or dielectric constant, and
ε ′′ is the imaginary part, or loss factor. The dielectric constant determines how
much of the incident energy is reflected at the air–sample interface and how much
enters the sample (for vacuum, ε ′ = 1); the loss factor measures the efficiency of the
absorbed microwave energy to be converted into heat [12]. The loss tangent (tan d
or dielectric loss) is the most important property in microwave processing; it
measures the ability of the matrix to absorb microwave energy and dissipate heat to
surrounding molecules, being responsible for the efficiency of microwave heating
[12, 13] As a result, a material with high loss factor and tan d combined with a
moderate value of ε ′ allows converting microwave energy into thermal energy.
The first factor one must consider when selecting microwave physical constants
is the solvent to be used. It is important to select a solvent with high extracting
power and strong interaction with the matrix and the analyte. Polar molecules
and ionic solutions (typically acids) strongly absorb microwave energy because of
the permanent dipole moment. On the other hand, when exposed to microwaves,
nonpolar solvents such as hexane will not heat up.
The degree of microwave absorption usually increases with the dielectric constant.
In Table 2.1, the physical parameters, including dielectric constant and dissipation
factors, are shown for commonly used solvents. A simple comparison between water
and methanol shows that methanol has a lesser ability to obstruct the microwaves as
they pass through but has a greater ability to dissipate the microwave energy into heat
[8]. The higher dielectric constant of water implies a significantly lower dissipation
factor, which means that the system absorbs more microwave energy than it can
dissipate. This phenomenon is called superheating: it occurs in the presence of water
in the matrix. This strong absorption provides an increase of the temperature inside
the sample, leading to the rupture of cells by the in situ water. In some cases it can
promote the degradation of the target compound or an “explosion” of solvent, and in
other cases it can increase the diffusivity of the target compound in the matrix [16].
Therefore, the microwave power must be sufficient to reach the boiling point of the
water or other solvent, setting the separation temperature.
The second factor to be considered is the solid matrix. Its viscosity affects its
ability to absorb microwave energy because it affects molecular rotation. When the
molecules are “locked in position” as viscous molecules, molecular mobility is
reduced, thus making it difficult for the molecules to align with the microwave field.
Therefore, the heat produced by dipole rotation decreases, and considering the
higher dissipation factor (d), the higher is this factor, the faster the heat will be
transferred to the solvent [11].
2.1.3 Heat Transfer in Microwave Heating
When the system is subjected solely to heating, then Eq. (2.4) can be solved by
itself. Thus, the initial condition needed to determine the unique solution of
Eq. (2.4) is the initial temperature of the system, given as
T(x, y, z, t) t = 0 = T0 (x, y, z ) (2.4)
The convective boundary condition at the material surfaces is given by Newton’s

law of cooling and is used as follows:
∂T
( )
h Ta − T n = a = k t
∂n n = a
(2.5)
And, the adiabatic boundary condition applied in the center of the substrate par-
ticles is
∂T
=0 (2.6)
∂n n=0
where n is the specific dimension, a is the boundary position, h is the convective

heat transfer coefficient, kt is the thermal conductivity, and Ta is the temperature of
the surrounding air.
Considering a transient heat transfer in an infinite slab, for one-dimensional flux,
the corresponding equation is
∂ 2T q ′′ 1 ∂T
+ = (2.7)
∂x 2 kt α ∂t
where x is the heat flux direction, q ′′ is the heat generation, kt is the thermal con-
ductivity, and a is the thermal diffusivity.
Food materials are, in general, poor electric insulators. They have ability to store
and dissipate electric energy when subjected to an electromagnetic field. Microwave
energy in itself is not thermal energy. The heating is a result of the electromagnetic
energy generated with the dielectric properties of the material combined with the
electromagnetic field applied. Dielectric properties play a critical role in determining
the interaction between the electric field and the matrices [17]. The rate of conversion
of electrical energy into thermal energy in the material is described by Chen
et al. [18]:
P = K . f ε ′ E 2 tan δ (2.8)
where P is the microwave power dissipation per volume unit, K is a constant, f

is the frequency applied, ε ′ is the absolute dielectric constant of the material, E is
the electric field strength, and tan δ is the dielectric loss tangent.
The distribution of the electric field depends on the geometry of the irradiated
object and its dielectric properties. The depth of penetration of a wave ( Dp ) can
also have an important role in the choice of the working frequency and depends on
the thickness of the matrix being treated. The energy absorption inside the solid
material causes an electric field that decreases with the distance from the material
surface. The penetration depth ( Dp ) is the distance from the material surface where
the absorbed electric field ( ε ) is reduced to 1/ ε of the electric field at the surface:
this corresponds to an energy loss of about 37% [19]. The penetration depth is
inversely proportional to the frequency and the dielectric properties of the material,
as shown by the following expression [20]:
c
Dp = 1/ 2
(2.9)
2π f ′ 2ε ′ ⎡ 1 + tan 2δ − 1⎤
⎣ ⎦
where c is the speed of light (m/s). This equation is approximated by the follow-
ing (Eq. (2.24)), when tan d << 1, which is usually the case:
λ0 ε r′
d= (2.10)
2πε r′′
where l0 is the wavelength in vacuum and d the approximate penetration depth.

The depth of penetration varies inversely with the loss factor and is even less when
the product is sensitive to microwaves. If the penetration depth of the microwave is
much less than the thickness of the material, only the surface is heated, and the rest
of the material is heated by conduction. For transparent media, that is, a loss factor
<0.01, the depth of penetration is not problematic and will dissipate the energy. The
presence of a standing wave will induce the creation of “hot spots” where the power
dissipated exceeds the heat transfer to cooler areas of the environment.
2.2 Heat and Mass Transfer: Balance Equations and Kinetics
Plant materials can be considered as porous media because of their similarities to

solid food that can be treated as hygroscopic and capillary-porous [21]. According
to Datta [22] the distinction between porous and capillary-porous is based on the
presence and size of pores. Generally, porous materials have pores ³ 10−7 m, whereas
for capillary-porous materials the pores are £ 10−7 m. The presence of pores makes
the water transport in these systems more intricate, because, in addition to the con-
tribution of molecular diffusion, the transport within the pores is also caused by
Knudsen diffusion (mean free path of molecules is long compared to the pore size),
surface diffusion, and hydrodynamic flow [21].
Considering the extraction process, microwaves are generally used in two
situations: (1) MAE that can be treated as a solid–solvent extraction, in which case
the equations developed by Takeuchi et al. [23] can be used, and (2) solvent-free MAE
(SFMAE), which can be treated as a two-step process in which in the first step,
system temperature in any given location is less than that of water evaporation, and
in the second step, the temperature at any given location is equal to the boiling tem-
perature; thus, the electromagnetic energy is entirely used to evaporate the water.
2.2.1 Heat and Mass Balance Equations for Solid–Liquid MAE
The mass transfer equations for solid–liquid extraction were presented by Takeuchi
et al. [23] for an isothermal process. The factors that control the extraction of a
solute from a matrix using MAE are the mass transfer rate of the solute from the
matrix to the solution phase and the strength of solute–matrix interactions. Although
the solubility of the solute in the solvent is recurrently indicated as a limiting factor,
it should not be so because the solvent-to-solid ratio is large enough to assure that
the extract–solvent mixture forms an infinite diluted solution.
The rate of dissolution of a solute into the extraction solvent is controlled by the
mass transfer rate of the solute from the solid matrix into the liquid. The transfer of
the solute inside the solid particle occurs because of the concentration gradient
in the solid–liquid interface, and it can be characterized by the effective diffusion.
The equation that describes this phenomenon is based on Fick’s law:
NC dCC
= − DBC (2.11)
AT dz
where NC is the rate of dissolution of the solute C in the solution (kg/s), AT is the
area of the solid–liquid interface (m2), DBC is the diffusivity of the solute in the solvent–
inert solid (m2/s), CC is the concentration of solute C in the solution (kg/m3), and z
is the distance inside the porous part of the solid matrix (m). The minus sign gives
a positive flux term because the gradient is negative (flow occurs down a concentration
gradient, from high to low concentration).
Diffusion coefficient data are necessary to make calculations. Diffusivities may

be determined experimentally or predicted. Orders of magnitude of diffusion
coefficients ( DBC ) for solids are 10−9 to 10−10 m2/s. When concerned with imperme-
able porous solids with fluid-filled pores, the effective (or apparent) diffusion
coefficient is used:
ε
DCBeff = DBC (2.12)
τ
where e is the void fraction or porosity of the solid and t is the tortuousness of the
pores.
On the surface of the solid particle, the transfer of the solute occurs simultane-
ously by molecular and turbulent transport. In this step, the mass transfer rate can be
expressed by the following equation:
VdCC
NC = V = AT K L (CCS − CC ) (2.13)
dt S
where K L is the mass transfer coefficient (m/s), CCS is the reference concentration
of the solute C in the solid surface (kg/m3), and CC is the concentration of the solute
C in the solution at time t (kg/m3).
Integrating Eq. 2.14 from t = 0 and CC = CC0 to t = t and CC = CC, we obtain:
CC dCC Ak t
∫CC 0 CCS − CC
= L
V ∫ t =0
dt (2.14)
⎛ kL A ⎞
CCS − CC −⎜ ⎟t
=e ⎝ V ⎠
(2.15)
CCS − CC 0
If pure solvent is used initially, CC0 = 0, and then
⎛ kL A ⎞
C −⎜ t
V ⎟⎠
1− C = e ⎝ (2.16)
CCS
⎛ −⎜ L ⎟ t ⎞
⎛ k A⎞
CC = CCS ⎜ 1 − e ⎝ V ⎠ ⎟ (2.17)
⎝ ⎠
2.2.2 Heat and Mass Balance Equations for SFMAE
In order to formulate the heat and mass balance, material will be considered, as
suggested by Navarrete et al. [24], as a capillary-porous media that includes the
insoluble solids, bound and free water, and air. Heat is generated and conducted in
the capillary-porous medium. The vapor phase forms an homogeneous system, and
heat convection can be neglected. Steam is removed from the system instanta-
neously, that is, no diffusion or convection was considered. The evaporation of
water consumed all heat generated in the system. MAE is considered to be per-
formed in a fixed bed formed by the plant material packed inside the extraction
vessel. During the extraction, system temperature will be equal to or less than the
boiling temperature. So long as the temperature in a given location of the bed did
not reach the boiling temperature, the general heat transfer equation or the thermal
conduction equation can be used to estimate the heat transfer flux and describes the
space and time behavior of the temperature field [24]:
∂T
rS CP − ∇ • (K t ∇T ) = P (2.18)
∂t
where rS represents the solid material apparent density (kg m−3), CP is the specific
heat capacity (J kg−1 K−1), and K t is the thermal conductivity (A V−1 m−1). T = T (x,
y, z, t) is the absolute temperature and P = P (x, y, z, t) is the microwave energy power
dissipated per volume unit; this corresponds to the heat generated by the interaction
between microwaves in the plant material. Note that the parameters rS , CP and K t
should be estimated for the lumped capillary-porous media as already described.
The moisture content varies during the extraction process, and these parameters
vary with the moisture of the system: for MAE these parameters are not constant.
Nonetheless, for other systems in which only heating is the important phenomenon,
these parameters are usually taken as constants that are independent of position,
time, and temperature, which simplifies the solution of the heat transfer equation.
According to Navarrete et al. [24], the time-average power dissipated in a plant
material per unit volume can be calculated from
1 2
P= ( K t + ωε oε ′′) E (2.19)
2
where w is the angular frequency of the electromagnetic wave, eo is the vacuum

permittivity (8.8542 × 10−12 F m−1), e is the dielectric loss factor, and E is the electric
field (V m−1).
After the system temperature has reached the boiling temperature, the energy
generated will be used for the evaporation of water. Therefore, the evaporation rate
will be given by Navarrete et al. [24]:
∂Cw
= Rw (2.20)
∂t
where Cw (kg m−3) is the water concentration per unit volume of extractor vessel and
Rw is the water evaporation rate (kg s−1 m−3)
So long as water is evaporating, the rate of evaporation can be estimated from
Navarrete et al. [24]:
P
Rw = (2.21)
λw
Equations 2.6 and 2.7 were proposed by Navarrete et al. [24] to describe the
SFME (solvent-free microwave extraction) of Lavandin essential oil. To solve Eqs.
(2.5), (2.6), and (2.7), the authors estimated the system properties using the equa-
tions of Datta [21, 22], Navarrete et al. [24], and Sihvola [25]. The specific heat of
the lumped system as a function of system moisture was estimated using [21]
CP = rS CPS (1 − j )+ rw CPwj Sw + rg CPgj (1 − Sw ) (2.22)
where CPg , CPS and CPw are the air, insoluble solid, and water specific heat, and
rg , rS and rw are the air, insoluble solid, and water densities. Sw is the amount of
water in pores and is generally referred to as the water saturation; it is calculated
from [21]
M w (1 − j )rS
Sw = (2.23)
(1 − M w )jrS
where M w is the plant material moisture, which is calculated from
CwV
Mw = (2.24)
CwV + (1 − M wo )mo
where M wo and mo are the initial moisture content of the plant material and the mass
of feed, respectively. j is the bed porosity and is calculated using [21]
rB (1 − M w )
j = 1− (2.25)
rS
where r B is the bed apparent density.
2.3 Important Parameters in Microwave-Assisted

Extraction and Mechanism of Action
The optimization of MAE conditions has been studied in several applications.

The efficiency of the process is directly related to the operation conditions selected.
Special attention should be given to usually studied parameters that may influence
the performance of MAE such as solvent composition, solvent-to-feed ratio, extrac-
tion temperature and time, microwave power, and the characteristics of the matrix
including its water content. Comprehension of the effects and interactions of these
factors on the MAE process is significant. Thus, this topic emphasizes some of the
parameters that affect MAE, presenting guidelines regarding the selection of proper
operation conditions, and also discusses the interaction between these parameters.
2.3.1 Effect of Solvent System and Solvent-to-Feed Ratio (S/F)
The most important factor that affects MAE process is solvent selection. A proper
solvent choice will provide a more efficient extraction process. Solvent selection
depends on the solubility of the compounds of interest, solvent penetration and its
interaction with the sample matrix and its dielectric constant [26], and the mass
transfer kinetics of the process [27]. The solvent should preferably have a high selec-
tivity toward the solutes of interest excluding undesired matrix components. Another
important aspect is that the optimal extraction solvents cannot be selected directly
from those used in conventional extractions: it depends on the capacity of the solvent
to absorb the microwave energy and consequently heat up [7, 8, 13, 28].
In general, the capacity of the solvent to absorb microwave energy is high when
the solvent presents high dielectric constant and dielectric loss [27]. Solvents that
are transparent to microwaves do not heat when submitted to them. Hexane is an
example of microwave-transparent solvent whereas ethanol is an excellent micro-
wave-absorbing solvent [13, 29]. Both polar and nonpolar solvents can be used in
MAE, and solvents such as ethanol, methanol, and water are sufficiently polar to be
heated by microwave energy [30]. In this context, the properties of the solvent can
be modified when combining different solvents, which allow varying the solvent
selectivity for different compounds [30]. The addition of salts to the mixture can
also increase the heating rate, because besides dipole orientation the ion conductiv-
ity is the main origin of polarization and corresponds to losses to heat in dielectric
heating [27]. Studies have shown that small amounts of water in the extracting sol-
vent make possible the diffusion of water into the cells of the matrix, leading to
better heating and thus facilitating the transport of compounds into the solvent at
higher mass transfer rates.
In the case of volatile compounds, the addition of a solvent with relatively low
dielectric properties can be used to ensure that the solvent temperature is kept lower
to cool off the solutes once they are liberated into the solvent [7]. Generally, hexane
is used for the extraction of volatile oils [13]. In addition, the solvent-free MAE
(SFMAE) process has been designed for aromatic herbs rich in volatile oils; in this
case, the moisture content within the plant matrix itself serves for extraction and no
solvent is used [29, 31].
Studies have reported that ethanol or water can be added into poor microwave
absorbers, such as hexane, to improve the extraction efficiency. One of the most
used solvent mixtures is hexane-acetone [8], and only a small amount of water
(about 10%) must be added in nonpolar solvents such as hexane, xylene, or toluene
to improve the heating rate [8]. Zhou and Lui [32] evaluated different mixtures of
ethanol and hexane in the extraction of solanesol from tobacco leaves; the 1:3 ratio
gave the best yield. Comparing isopropanol and hexane for rice bran oil extraction,
hexane at 40°C extracted approximately 40% more oil than isopropanol. Although
by increasing the temperature hexane did not extract significantly more amount of
oil, isopropanol extracted about 25% more rice bran oil at 120°C [33].
Some authors studied the use of combined solvents in MAE according to the
polarity of the target compounds. A methanol–water (85:15) combination proved to
be a good solvent for MAE of gymnemagenin from Gymnema sylvestre R. Br.
Higher water concentration reduced the extraction yield because high water content
increases the mixture polarity to a degree where it is no longer is favorable for
extraction. The same was observed by Talebi et al. [34] when extracting paclitaxel
from Taxus baccata: a methanol–water (90:10) mixture was the best combination.
Song et al. [35], extracting sweet potato leaves, found that 60–80% (v/v) ethanol
concentration in water was optimal within proportions of 40% and 80% (v/v).
The solvent-to-solid (feed) ratio (S/F) is an important parameter to be optimized.
The solvent volume must be sufficient to guarantee that the entire sample is immersed
in the solvent throughout the entire irradiation process, especially when using a
matrix that will swell during the extraction [8, 13, 29].
In conventional extractions, the use of large volumes of solvent increases the
extraction recovery. Studies reported that the extraction solution must not exceed
30–34% (w/v) [8]. In many applications a ratio 10:1 (ml/mg) to 20:1 (ml/mg) was
found to be optimal [34, 36]. In addition, the solvent volume is an important factor
to be considered because too much of the extracting solvent means more energy and
time is required to condense the extraction solution in the later step and purification
process. On the other hand, MAE may give lower recoveries because of nonuniform
distribution and exposure to microwaves [37].
In some cases, small amounts of solvent are sufficient to extract the compounds
of interest. The phenol and methylphenol extracted from oils had optimal conditions
when S/F reached 2 [38]. A different behavior was observed in the MAE of artemisi-
nin from Aretimisia annua L.: a higher extraction rate was achieved by a greater
amount of solvent [39]. In Ganoderma atrum, the yield of triterpenoid saponins
increased with the increase of amount of solvent until the S/F reached 25, and then
it decreased rapidly [40].
2.3.2 Effect of Extraction Time and Cycle
In MAE the period of heating is another important factor to be considered. Extraction

times in MAE are very short compared to conventional techniques and usually vary
from a few minutes to a half-hour, avoiding possible thermal degradation and oxida-
tion [20, 28], which is especially important for target compounds sensitive to over-
heating of the solute–solvent system. Overheating occurs because of the high
dielectric properties of the solvent, especially ethanol and methanol, and further
dilution with water that increases the heat capacity of the solvent combination [7].
Higher extraction time usually tends to increase the extraction yield. However, this
increase was found to be very small with longer time [41]. Irradiation time is also
influenced by the dielectric properties of the solvent. Solvents such as water, ethanol,
and methanol may heat up tremendously on longer exposure, thus risking the future
of thermolabile constituents [13].
Occasionally, when longer extraction time is required, the samples are extracted
in multiple steps using consecutive extraction cycles, which are also an example of
the use of a larger amount of solvent and higher microwave application time [28,
42]. In this case, the fresh solvent is fed to the residue and the process is repeated to
guarantee the exhaustion of the matrix. With this procedure, the extraction yield is
enhanced, avoiding long heating [7, 28]. The number of process cycles will depend
on the type of matrix and the solute. According to Li et al. [43], three cycles of
7 min were appropriate for MAE of triterpene saponins from yellow horn, whereas
in optimization of triterpenoid saponins MAE from Ganoderma atrum, cycles of
5 min each were recommended [26]. Yan et al. [44] found that three extraction
cycles of 5 min each are optimal for extracting astragalosides from Radix astragali.
They also found that increasing the irradiation time from 1 to 5 min increases the
extraction yield rapidly; extraction reaches its maximum at 5 min, and then the
yields decreased with the extension of the irradiation time. In the case of flavonoids
extraction from R. astragali, there was an increase in yield with time up to an expo-
sure of 25 min and then the extraction yield started to decrease [42]. In the work of
Chen et al. [26] it was observed that triterpenoid saponins yield from Ganoderma
atrum reached its maximum at 20 min; after this time, the target compounds easily
decomposed because of long exposure to high temperature. The same behavior was
found by Song et al. [35].
2.3.3 Effect of Microwave Power and Extraction Temperature
Microwave power and temperature are interrelated because high microwave power
can bring up the temperature of the system and result in the increase of the extraction
yield until it becomes insignificant or declines [4, 42, 45]. It is known that the tem-
perature is controlled by incident microwave power that controls the amount of energy
provided to the matrix, which is converted to heat energy in the dielectric material.
At high temperatures the solvent power increases because of a drop in viscosity
and surface tension, facilitating the solvent to solubilize solutes, and improving
matrix wetting and penetration [13, 43, 46]. In addition, when MAE is performed in
closed vessels, the temperature may reach far above the boiling point of the solvent,
leading to better extraction efficiency by the desorption of solutes from actives sites
in the matrix [8]. However, Routray and Orsat [7] state that the efficiency increases
with the increase in temperature until an optimum temperature is reached and then
starts decreasing with the further increase in temperature: this happens because the
selection of ideal extraction temperature is directly linked with the stability and,
therefore, with the yield of the target compound.
Microwave power is directly related to the quantity of sample and the extraction
time required. However, the power provides localized heating in the sample, which
acts as a driving force for MAE to destroy the plant matrix so that the solute can
diffuse out and dissolve in the solvent. Therefore, increasing the power will generally
improve the extraction yield and result in shorter extraction time [4, 28]. On the
other hand, high microwave power can cause poor extraction yield because of the
degradation of thermally sensitive compounds. Also, rapid rupture of the cell wall
takes place at a higher temperature when using higher power, and as a result impuri-
ties can also be leached out into the solvent together with the desired solute [13].
Therefore, it is important to properly select the MAE power to minimize the time
needed to reach the set temperature and avoid a “bumping” phenomenon in
temperature during the extraction [8]. Moreover, the overexposure to microwave
radiation, even at low temperature or low operating power, was found to decrease the
extraction yield because of the loss of chemical structure of the active compounds.
Knowing that power level alone does not gives sufficient information about the
microwave energy absorbed into the extraction system, Alfaro et al. [47] created a
term to study the effect of microwave power on MAE: energy density, defined as the
microwave irradiation energy per unit of solvent volume for a given unit of time
(W/ml). According to Li et al. [43], the energy density should be considered as a
parameter as power level alone. In this study, the anthocyanin extraction rates from
grape peel were different under the same microwave power level, extraction time,
and S/F because the energy density levels were different.
Raner et al. [48] reported that variation of power from 500 to 1,000 W had no
significant effect on the yield of flavonoids. The decrease in extraction yield was
found at temperatures higher than 110°C because of instability of flavonoids and
consequent thermal degradation [42]. In another case, higher microwave power led
to thermal degradation of phenols when it was higher than 350 W (between 150 and
550 W) [35]. The temperature behavior was the same in other studies. In extracting
astragalosides from Radix astragali, Yan et al. [44] also found that yield increased
remarkably with temperature increase from 50°C to 70°C; above 70°C, the yields of
astragalosides increased slowly and even decreased.
2.3.4 Effect of Contact Surface Area and Water Content
Not only the parameters already discussed but the characteristics of the sample also
affect the MAE process. It is known that in a higher contact surface area the extrac-
tion efficiency increases. Also, finer particles allow improved or much deeper pen-
etration of the microwave [49]. On the other hand, very fine particles may pose
some technical problems; consequently, centrifugation or filtration is applied to pre-
pare the matrix [13, 29]. In the preparation step the sample is grinded and homog-
enized to increase the contact area between the matrix and the solvent. The particle
sizes are usually in the range of 100 mm to 2 mm [8]. In some cases soaking of the
dried plant material in the extracting solvent before MAE has resulted in improved
yield. This procedure is called pre-leaching extraction [13].
In many cases the extraction recovery is improved by the matrix moisture, which
acts as a solvent. The moisture in the matrix is heated, evaporated, and generates
internal pressure in the cell, which ruptures the cell to release the solutes, hence
improving the extraction yield [31]. When increasing the polarity of the solvent,
water addition has a positive effect on the microwave-absorbing ability and, hence,
facilitates the heating process [8, 28]. Moreover, the additional water promotes
hydrolyzation, thus reducing the risk of oxidation of the compounds [41].
In extraction of astragalosides from Radix astragali, extraction efficiency was
improved by the addition of water. The possible reason for the increased efficiency
is the increase in swelling of plant material by water, which enhances the contact
surface area between the plant matrix and the solvent [44].
2.3.5 Effect of Stirring
The effect of stirring is directly related to the mass transfer process in the solvent
phase, which induces convection in the headspace. Therefore, equilibrium between
the aqueous and vapor phases can be achieved more rapidly. The use of agitation in
MAE accelerates the extraction by enhancing desorption and dissolution of active
compounds bound to the sample matrix [50]. Through stirring, the drawbacks of the
use of low solvent-to-solid ratio (S/F) can be minimized, together with the minimi-
zation of the mass transfer barrier created by the concentrated solute in a localized
region resulting from insufficient solvent [28]. In the work by Kovács et al. [51] it
is possible to observe the difference between suspensions with and without stirring.
The authors found that when the suspensions were agitated with magnetic stirrers
the temperature reached its maximum value within a shorter time, and the tempera-
ture differences inside individual vessels were not significant.
2.4 Comparison of Microwave-Assisted Extraction (MAE) with

Other Solid–Liquid Extraction Techniques
To introduce bioactive plant extracts in pharmaceutical and cosmetic formulations,

industries are looking for green and efficient extraction processes free of toxic sol-
vents. Methodologies using biodegradable and nontoxic solvents such as water and
ethanol are being developed [52].
The traditional techniques of solvent extraction of plant materials are based on
the correct choice of solvents and the use of heat or/and agitation to increase the
solubility of the desired compounds and improve the mass transfer. Soxhlet extrac-
tion is the most common and is still used as a standard in all cases [53]. As a result
of several secondary metabolites, the development of high performance and rapid
extraction methods is an absolute necessity [54]. The new extraction techniques
with shortened extraction time, reduced solvent consumption, increased pollution
prevention, and with special care for thermolabile constituents have gained atten-
tion. In the many published papers comparing MAE with other advanced and con-
ventional extraction methods, MAE has been accepted as a potential and powerful
alternative for the extraction of organic compounds from plant materials [55].
The ideal extraction technology depends on the type of compound to be extracted,

whereas the extraction method efficiency is based on the highest recovery, espe-
cially of the effective constituents, the shortest processing time, the lowest produc-
tion cost, and use of minimum organic solvent [56]. There have been numerous
reviews and research on the advances of different extraction techniques, comparing
their results. In the extraction of bioactive compounds from plants, MAE was
reported to be more efficient compared to conventional techniques such as Soxhlet
and advanced methods of extraction including ultrasound-assisted extraction (UAE),
pressurized liquid extractions (PLE), and supercritical fluid extraction (SFE), which
have emerged as energy-saving technologies. Over the years the procedures based
on MAE have replaced some conventional extraction methods and have been
adopted over decades in laboratories and industry.
In addition, the progress in microwave extraction gave rise to other categories of
techniques to improve its performance: (1) microwave-assisted distillation (MAD) for
the isolation of essential oils from herbs and spices [57]; (2) microwave hydrodiffusion
and gravity (MHG), a combination of microwave heating and distillation at atmospheric
pressure that requires less energy and no solvent and simply combines microwaves and
earth gravity at atmospheric pressure [58]; (3) vacuum microwave hydrodistillation
(VMHD), which uses pressures between 100 and 200 mbar to evaporate the azeotropic
mixture of water–oil from the biological matrix [59]; (4) microwave-integrated Soxhlet
extraction (MIS), a combination of microwave heating and Soxhlet [60]; and (5) sol-
vent-free microwave extraction (SFME), based on the combination of microwave heat-
ing and distillation, which is performed at atmospheric pressure [61]. If these techniques
are explored scientifically, they can be proven to be efficient extraction technologies for
ensuring the quality of herbal medicines worldwide [13].
As already mentioned, MAE is increasingly employed in the extraction of natu-
ral products as an alternative to traditional techniques of extraction for several rea-
sons: reduced extraction time, reduced solvent consumption, and less environmental
pollution as a result of increased efficiency and clean transfer of energy to the
matrix; improved extraction yield and product quality, because materials can be
rapidly heated, and often processed at lower temperatures; up to 70% energy saving
compared to conventional energy forms from the high energy densities and the
direct absorption of energy by the materials; compact systems, as small as 20% of
the size of conventional systems; and selective energy absorption resulting from the
dielectric properties of the material and applicator design [52, 55, 62].
On the other hand, some disadvantages can also be mentioned: additional
filtration or centrifugation is necessary to remove the solid residue after the process;
the efficiency of microwaves can be poor when the target compounds or solvents are
nonpolar, or when they are volatile; and the use of high temperatures that can lead
to degradation of heat-sensitive bioactive compounds [63].
Considering these advantages and drawbacks of MAE compared to other tech-
niques, a discussion on MAE performance compared to conventional and advanced
techniques as Soxhlet, SFE, UAE, and PLE is appropriate. Table 2.2 presents their
advantages and drawbacks; and Table 2.3 shows studies comparing the extraction
technologies and their respective optimization.
Table 2.2 Comparison of traditional and advanced extraction techniques for analytical-scale extraction (adapted from Ref. 8 and 64)
Extraction technique
Microwave-assisted Ultrasound-assisted Pressurized solvent
Soxhlet extraction (MAE) extraction (UAE) Supercritical fluid extraction (SFE) extraction (PLE)
Brief Sample is placed in a Sample is immersed in a Sample is immersed in Sample is loaded in a high-pressure vessel Sample and solvent are
descrip- glass fiber thimble microwave-absorbing solvent in a vessel and extracted with supercritical fluid heated and pressur-
tion and by using a solvent in a closed and submitted to (most commonly carbon dioxide at ized in an extraction
Soxhlet extractor, vessel and irradiated ultrasonic using US pressures of 150–450 bar and tempera- vessel; when the
the sample is with microwave energy probe or US bath tures of 40°–150°C). The analytes are extraction is finished,
repeatedly perco- collected in a small volume of solvent, the extract is
lated with recon- in a separator or onto a solid-phase automatically
densed vapors of the trap, which is rinsed with solvent in a transferred into a
solvent subsequent step vial
Extraction 3–48 h 3–30 min 10–60 min 10–60 min 5–30 min
time
Sample size 1–30 g 1–10 g 1–30 g 1–5 g 1–30 g
Solvent use 100–500 ml 10–40 ml 30–200 ml 2–5 ml (solid trap) 10–100 ml
5–20 (liquid trap)
Investment Low Moderate Low High High
Advantages Easy to handle, no Fast and multiple Easy to use, multiple Fast extraction, low solvent consumption, Fast extraction, no
filtration necessary, extraction, easy to extractions concentration of the extract, no filtration necessary,
high matrix capacity handle, moderate filtration necessary, possible high low solvent
solvent consumption, selectivity, low temperatures, no use of consumption,
elevated temperatures toxic solvents, automated systems elevated temperature,
automated systems
Drawbacks Long extraction time, Extraction solvent must Large solvent volume, Many parameters to optimize, especially Possible degradation of
large solvent absorb microwave filtration step analyte collection thermolabile
volume, cleanup energy, filtration step required, repeated analytes, cleanup
step is needed required, waiting time for extractions may be step is needed
the vessels to cool down required
32
Table 2.3 Comparison on the extraction yield between MAE and other techniques
Operational conditions: type of solvent(s), solvent to feed ratio (S/F),
temperature (T), pressure (P), time (t), raw material moisture content (h), Bioactive compound extracted and
rotation (r), frequency (f), power (Pw), flow rate (v), power to feed ratio extraction yield (dry basis, db; wet
Plant material (P/F), humidity (h) basis, wb) References
a
Sweetgrass leaves MAE: 5,8-Dihydroxycoumarin (0.42% db ) [65]
(Hierochloe odorata L.) Pw = 200 W; s = acetone; S/F = 10; T = 80 C; 5-Hydroxy-8-O-b d-glucopyranosyl-
P = Patm; t = 15 min; one-step extraction benzopyranone (0.11% dba)
SFE: 5,8-Dihydroxycoumarin (0.49% dba)
Two-step: 5-hydroxy- 8-O-b - d-glucopyranosyl-
(1) = 35 MPa; T = 40 C benzopyranone (0.06% dba)
(2) = P = 25Mpa; T = 40 C
S = ethanol (20%); t = 2 h; v = 0.5 l/min
Soxhlet: 5,8-Dihydroxycoumarin (0.46% dba)
S/F = 50; s = acetone; t = 6 h 5-Hydroxy-8-O-b -d-glucopyranosyl-
benzopyranone (0.08% dba)
Artemisia annua L. MAE: Artemisinin (92.1% dba) [66]
Pw = 650 W; s = solvent oil; S/F = 15; T = ambient;
t = 12 min
SFE: Artemisinin (33.2% dba)
P = 30 MPa; s = CO2; S/F = 6; T = 35 C; t = 2.5 h
Soxhlet: Artemisinin (60.4% dba)
s = Solvent oil; S/F = 11.67; T = 35 C; t = 6 h
Licorice roots MAE: Glycyrrhizic acid –GA (2.26%a) [67]
(Glycyrrhizia glaubra) Pw = 700 W; s = ethanol; S/F = 10; T = 85 –90 C;
t = 4 min
US: Glycyrrhizic acid –GA (2.26%a)
s = ethanol; S/F = 10; t = 20.5 h
Soxhlet: Glycyrrhizic acid –GA (2.5%a)
P.C. Veggi et al.
s = ethanol; S/F = 10; t = 10 h

2

a
Green tea leaves MAE: Tea polyphenols (30% ) [36]
Pw = 700 W; s = ethanol: water (1:1 v/v); S/F = 20; Tea caffeine (4%a)
T = 20 C; t = 4 min
UAE: Tea polyphenols (28%a)
s = ethanol: water (1:1 v/v); S/F =; T = 20 C–40 C; Tea caffeine (3.6%a)
t = 90 min
Heat reflux extraction: Tea polyphenols (28%a)
s = ethanol: water (1:1 v/v); S/F =; T = 85 C; Tea caffeine (3.6%a)
t = 45 min
Grapefruit MAE: Pectin (27.81% dba) [68]
Pw = 0.9 kW; s = water; S/F = 30; T = 20 C; t = 6 min
UAE: Pectin (17.92% dba)
s = water; S/F = 30; T = 70 C; t = 25 min

UAE + MAE: Pectin (31.88% dba)
Pw = 0.45 kW; S/F = 30;
t = 30 min (UAE) and 10 min (MAE)
Heat batch: Pectin (19.16% dba)
s = water; S/F = 30; T = 90 C; t = 90 min
Ganoderma atrum MAE: Global yield (5.11% dba) [69]
s = ethanol: water (9.5: 0.5 v/v); S/F = 25; T = 90 C;
t = 5 min
UAE: Global yield (1.72% dba)
s = ethanol: water (9.5: 0.5 v/v); S/F = 25; t = 30 min;
f = 33 kHz
SFE: Global yield (1.52% dba)
P = 25 MPa; T = 55 C; s = CO2 + ethanol; t = 3 h
Shaking: Global yield (2.58% dba)
s = ethanol: water (9.5: 0.5 v/v); t = 3 h
HRE: Global yield (2.22% dba)
33
s = ethanol (9.5: 0.5 v/v); S/F = 25; T = 95 C; t = 1 h

(continued)
Table 2.3 (continued)
34

a
Yellow horn MAE: Global yield (11.62% db ) [43]
(Xanthoceras Pw = 900 W; s = ethanol:water (40: 60 v/v); S/F = 30;
sorbifolia Bunge.) T = 50 C; t = 7 min × 3 cycles
Pw = 250 W; s = ethanol:water (40: 60 v/v); S/F = 30;
T = 50 C; t = 60 min × 3 cycles
HRE: Global yield (10.82% dba)
Pw = 800 W; s = ethanol: water (40: 60 v/v); S/F = 30;
T = 50 C; t = 90 min × 3 cycles
Turmeric plant MAE: Curcumin (90.47% dba) [70]
(Curcuma longa L.). Pw = 60 W; s = acetone; S/F = 3; T = 50 C; t = 5 min
UAE: Curcumin (71.42% dba)
Pw = 150 W; s = acetone; S/F = 3; T = 21 C; t = 5 min
Soxhlet: Curcumin (2.10% dba)
s = acetone; S/F = 5; t = 8 h
SFE: Curcumin (69.36% dba)
P = 30 MPa; s = CO2+ ethanol (10%); T = 50 C;
t = 240 min; v = 5 ml/min
Silybum marianum (L.) MAE: Silybinin (1.37% dba) [56]
(milk thistle) Pw = 600 W; s = ethanol: water (80:20 v/v); S/F = 25;
t = 2 min × 6 cycles
Soxhlet: Silybinin (1.09% dba)
s = ethanol: water (80:20 v/v); S/F = 100; t = 12 h
Stirring: Silybinin (0.48% dba)
P.C. Veggi et al.
Maceration: Silybinin (0.36% dba)

2
b
Coriandrum sativum MAE: Phenolics content (0.082% db ) [71]
Pw = 200 W; s = ethanol: water (50:50 v/v); S/F = 20;
T = 50 C, t = 18 min
UAE: Phenolics content (0.041% dbb)
s = ethanol: water (50:50 v/v), S/F = 10; t = 30 min
Cinnamomum MAE: Phenolics content (1.679% dbb) [71]
zeylanicum Pw = 200 W; s = ethanol: water (50:50 v/v); S/F = 20;
T = 50 C, t = 18 min
Cuminum cyminum MAE: Phenolics content (1.159% dbb) [71]

Pw = 200 W; T = 50 C, s = ethanol: water (50:50 v/v);
S/F = 20; t = 18 min
Crocus sativus MAE: Phenolics content (2.939% dbb) [71]
Pw = 200 W; T = 50 C, s = ethanol: water (50:50 v/v); S/F = 20; t = 18 min
(continued)
35
36

Sea buckthorn MHG: Isorhamnetin 3-O-rutinoside (0.123% [2]
dba)
(Hippophae rhamnoides) Pw = 400 W; t = 15 min; h = 57% Isorhamnetin 3-O-glucoside (0.097% dba)
Quercetin 3-O-Glucoside (0.025% dba)
Isorhamnetin (0.00084% dba)
Agitated: Isorhamnetin 3-O-rutinoside (0.187%
dba)
s = methanol: water (80:20 v/v); S/F = 10; t = 8 min Isorhamnetin 3-O-glucoside (0.162% dba)
Quercetin 3-O-Glucoside (0.016% dba)
Isorhamnetin (0.00064% dba)
Cranberry press cake MAE: Quercetin (0.1272% dba) [72]
s = ethanol; S/F = 5.7; T = 125 C; t = 10 min
Stirring: Quercetin (0.1537% dba)
s = ethanol; S/F = 5; t = 2 h
Morinda citriflora (roots) MAE: Global yield (95.91% dba) [73]
Pw = 720 W; s = ethanol: water (80:20 v/v); S/F = 100;
T = 60 C; t = 15 min
s = ethanol; S/F = 100; T = 60 C; t = 60 min
Maceration: Global yield (63.33% dba)
s = ethanol; S/F = 100; t = 3 days
Soxhlet: Global yield (97.74% dba)
s = ethanol; S/F = 100; T = 100 C; t = 4 h
P.C. Veggi et al.
2
a
Soybean germ MAE: Global yield (16.5% wb ) [74]
S/F = 17.5; T = 120 C; t = 0.5 h
MAE + UAE: Global yield (14.1% wba)
Pw = 60 W (UAE) and 100 W (MAE); S/F = 5;
T = 45 C; t = 1 h
Soxhlet: Global yield (8.65% wb)
s = hexane; S/F = 6.67; t = 4 h
Lavandula angustifolia MASD: Monoterpenes (3.54% dba) [75]
Mill., Lamiaceae Pw = 500 W; s = water; S/F = 4; t = 10 min Oxygenated monoterpenes (78.29% dba)
(lavender flowers) Sesquiterpenes (2.77% dba)
Global yield (8.86% dba)
SD: Monoterpenes (4.92% dba)

s = water; S/F = 4; t = 90 min Oxygenated monoterpenes (75.14% dba)
Sesquiterpenes (2.87% dba)
Caraway (Carum carvi MDG: Global yield (2.59% dba) [76]
L.) Pw = 100 W; t = 45 min Carvone (67.59% dba)
Limonene (30.10% dba)
Hydrodistillation: Global yield (2.54% dba)
S/F = 5; t = 300 min Carvone (66.89% dba)
Limonene (30.30% dba)
Tomato MAE: Total phenolic contents (0.646% dbb) [77]
Pw = 100 W; s = methanol; S/F = 50; t = 45 min
Shaker: Total phenolic contents (0.603% dbb)
s = ethanol: water (60: 40 v/v); S/F = 50; T = 45 C;
r = 400 rpm; t = 15 h
(continued)
37
38

a
Foeniculum vulgare MWHD: Global yield (1.14% db ) [78]
Miller (seeds) Pw = 300 W; s = water; S/F = 2; T = 100 C; t = 200 s
HD: Global yield (0.265% dba)
Pw = 300 W; s = water; S/F = 8; t = 319 s; T = 100 C;
r = 50 rpm
Iochroma gesnerioides MAE: Withaferin A (0.48% dba) [79]
(leaves) Pw = 25 W; s = methanol; S/F = 50; t = 40 s Iochromolide (0.85% dba)
Withacnistin (0.39% dba)
Soxhlet: Withaferin A (0.41% dba)
(1) s = water; S/F = 6; t = 15 min Iochromolide (0.81% dba)
(2) s = methanol; S/F = 100; t = 6 h Withacnistin (0.38% dba)
Xanthoceras sorbifolia MAE: Triterpene saponins (11.62% wba) [43]
Bunge. (yellow horn) Pw = 900 W; s = ethanol: water (40: 60 v/v); S/F = 30; T = 50 C;
UAE: Triterpene saponins (6.78%a)
Pw = 250 W; s = ethanol: water (40: 60 v/v); S/F = 30; T = 50 C;
Reflux: Triterpene saponins (10.82%a)
Pw = 800 W; s = ethanol: water (40: 60 v/v); S/F = 30;
T = 50 C; t = 90 min × 3 cycles
Ocimum SFME: Eugenol (43.2% wba) [80]
Basilicum L. (basil) Pw = 500 W; T = 100 C; t = 30 min Linalool (25.3% wba)
Global yield (0.029% wba)
HD: Eugenol (11.0% wba)
s = water; S/F = 12; T = 100 C; t = 4.5 h Linalool (39.1% wba)
P.C. Veggi et al.

2
Mentha crispa L. (garden SFME: Limonene (9.7% wba) [80]

mint) Pw = 500 W; T = 100 C; t = 30 min Carvone (64.9% wba)
HD: Limonene (20.2% wba)
s = water; S/F = 12; T = 100 C; t = 4.5 h Carvone (52.3% wba)
Thymus vulgaris L. SFME: g-Terpinene (17.1% wba) [80]
(thyme) Pw = 500 W; T = 100 C; t = 30 min Eugenol (51.0% wba)
HD: g-Terpinene (22.8% wba)
s = water; S/F = 12; T = 100 C; t = 4.5 h Eugenol (40.5% wba)
Elletaria cardamomum SFME: Global yield (2.70% dba) [81]
L. Pw = 390 W; T = 100 C; h = 67%; t = 75 min

(cardamom) HD: 26.23 1,8-Cineole
s = water; S/F = 10; T = 100 C; t = 6 h 5.29 Linalool
2.60 Terpin-4-ol
3.88 a-Terpineol
3.63 Linalyl acetate
45.45 a -Terpinyl acetate
Gymnema sylvestre MAE: Gymnemagenin (4.3% dba) [82]
R. Br. Pw = 280 W; s = methanol: water (85: 15 v/v); S/F = 25;
t = 6 min
Reflux: Gymnemagenin (3.3% dba)
s = methanol: water (85: 15 v/v); S/F = 100; T = 95 C;
t=6 h
Maceration: Gymnemagenin (1.7% dba)
s = methanol: water (85: 15 v/v); S/F = 100; t = 24 h
Stirring: Gymnemagenin (2.2% dba)
39
s = methanol: water (85: 15 v/v); S/F = 100; t = 24 h

(continued)
40

(Melilotus officinalis MAE: Coumarin (0.3978% db) [83]
(L.) Pallas) Pw = 100 W; s = water: ethanol (50: 50 v/v); S/F = 20; T = 50 C; O-Coumaric acid (0.1257% dba)
(yellow sweet clover) t = 5 min × 2 cycles Melilotic acid (0.9052% dba)
USAE: Coumarin (0.3569% dba)
s = water: ethanol (50: 50 v/v); S/F = 20; t = 60 min O-Coumaric acid (0.1269% dba)
Melilotic acid (0.8092% dba)
Soxhlet: Coumarin (0.2156% dba)
s = ethanol: water (95: 5 v/v); S/F = 16.67; t = 8 h O-Coumaric acid (0.0708% dba)
Melilotic acid (0.6314% dba)
Salvia miltiorrhiza MAE: Tanshinone IIA (0.29% dba) [84]
Bunge. (dried root) s = ethanol: water (95: 5 v/v); S/F = 10; T = 80 C; Cryptotanshinone (0.23% dba)
t = 2 min Tanshinone I (0.11% dba)
Reflux: Tanshinone IIA (0.25% dba)
s = ethanol: water (95: 5 v/v); S/F = 10; t = 45 min Cryptotanshinone (0.24% dba)
Tanshinone I (0.11% dba)
UAE: Tanshinone IIA (0.28% dba)
Soxhlet: Tanshinone IIA (0.33% dba)
P.C. Veggi et al.
2
a
Radix astragali (dried MAE: Astragalosides I (0.0788% db ) [44]
root) Pw = 700 W; s = ethanol: water (80:20 v/v); S/F = 25; T = 70 C; Astragaloside II (0.0351% dba)
t = 5 min × 3 cycles Astragaloside III (0.0206% dba)
Astragaloside IV (0.0278% dba)
Soxhlet: Astragalosides I (0.770% dba)
s = ethanol: water (80:20 v/v); S/F = 20; T = 90 C; Astragaloside II (0.347% dba)
t=4 h Astragaloside III (0.193% dba)
Reflux: Astragalosides I (0.761% dba)
s = ethanol: water (80:20 v/v); S/F = 20; T = 90 C; Astragaloside II (0.352% dba)
t=1 h Astragaloside III (0.203% dba)

UAE: Astragalosides I (0.519% dba)
Pw = 100 W; s = ethanol: water (80:20 v/v); S/F = 20; Astragaloside II (0.302% dba)
t = 40 min Astragaloside III (0.190% dba)
Maceration: Astragalosides I (0.411% dba)
s = ethanol: water (80:20 v/v); S/F = 20; t = 12 h Astragaloside II (0.299% dba)
Astragaloside III (0.166% dba)
Sweet potato [Ipomoea MAE: Total phenolics (6.115% dbb) [35]
batatas (L.) Lam.] Pw = 123 W; s = ethanol: water (53: 47 v/v); S/F = 25;
t = 2 min
CSE: Total phenolics (5.969% dbb)
s = ethanol: water (60: 40 v/v); S/F = 30; t = 120 min
(continued)
41
42

a
Tobacco leaves MAE: Solanesol (0.91% db ) [32]
Pw = 700 W; s = hexane: ethanol (1: 3 v/v) +
NaOH (0.05 mol/l); S/F = 10; t = 40 min
HRE: Solanesol (0.87% dba)
s = hexane: ethanol (1: 3 v/v) + NaOH (0.02 mol/l);
S/F = 10; T = 60 C; t = 180 min
Lavandula angustifolia MSD: 1,8-Cineole (14.40% dba) [85]
Mill., Lamiaceae Pw = 200 W; v = 8 g/min; t = 6 min Linalool (42.52% dba)
(lavender flowers) Global yield (2.7% dba)
SD: 1,8-Cineole (13.71% dba)
t = 30 min Linalool (40.43% dba)
Radix astragali (root of MAE: Flavonoids (0.1190%a) [42]
Astragalus; Huangqi) s = ethanol: water (95: 5 v/v); S/F = 25; T = 110 C;
Soxhlet: Flavonoids (0.1292%a)
s = methanol; S/F = 25; T = 85 C; t = 4 h
UAE: Flavonoids (0.0736%a)
s = methanol; S/F = 20;T = 60 C; t = 30 min × 2 cycles
HRE: Flavonoids (0.0934%a)
s = ethanol: water (90: 10 v/v); S/F = 25; T = 75 C;
t = 2 h × 2 cycles
P.C. Veggi et al.
2
a
Yellow onion VMHG: Quercetin (0.662%db ) [86]
Pw = 500 W; P = 700 mbar; P/F = 1 W/g; T = 81 C; Global yield (3.18% dba)
t = 26 min; h = 84.5%
MHG: Quercetin (0.283%dba)
P = 1 bar; T = 100 C; t = 23 min; h = 84.5%
CSE: Quercetin (0.890% dba)
s = methanol: water (80: 20 v/v); S/F = 10;
r = 8,000 rpm; t = 5 min
HRE heat reflux extraction, MHG microwave hydrodiffusion and gravity, MASD microwave-accelerated steam distillation, SD steam distillation
SFME solvent-free microwave extraction, MDG microwave dry-diffusion and gravity, MWHD microwave-assisted hydrodistillation
HD hydrodistillation, USAE Soxhlet extraction, ultrasound-assisted extraction, MSD microwave steam distillation
VMHG vacuum microwave hydrodiffusion and gravity, CSE conventional solvent extraction
a
Yield (%) = g compound per 100 g sample
b
Yield (%) = g gallic acid equivalent (GAE) per 100 g mass of sample
Adapted from Eskilsson and Bjöklund [8]; Chemat et al. [64]
43
2.4.1 MAE Versus Soxhlet
Soxhlet is the typical technique and the main reference for evaluating the perfor-
mance of other solid–liquid extraction methods as it has long been one of the most
used solid–liquid extraction techniques. In Soxhlet extraction the solid material
containing the solutes is placed inside a thimble holder, which is connected to a
flask containing the extraction solvent, and submitted to reflux. After this process,
the extract is concentrated by evaporation of the solvent [87]. This method has a
large dependence on plant characteristics and particle size, as the internal diffusion
may be the limiting step during extraction, and extraction and evaporation tempera-
tures affect the quality of the final products [31].
It is a general and well-established technique, which surpasses in performance
other conventional extraction techniques except, in a limited field of applications,
the extraction of thermolabile compounds. Furthermore, it presents other disadvan-
tages such as poor extraction of lipids, long operation time, high solvent consump-
tion, and operation at the solvent’s boiling point [88]. The advantages of this method
include no requirement of a filtration step after leaching and the displacement of
transfer equilibrium by repeatedly bringing fresh solvent into contact with the solid
matrix [31, 88].
Studies show that MAE allows the reduction of time and solvent consumption,
as well as improvement in global yield. Kaufmann et al. [89], extracting whitano-
lides from Lochroma gesneroides, showed a drastic reduction in solvent usage
(5 vs. 100 ml) and in extraction time (40 s vs. 6 h). Another study concluded that the
same quantity and quality of tanshiones from Salvia miltiorrhiza Bunge was
obtained with 2 min of MAE and 90 min of Soxhlet [90]. Higher yield was obtained
when extracting artemisinin from Artemisia annua L. by MAE; in 12 min, 92.1% of
artemisinin was recuperated by MAE whereas several hours were needed by Soxhlet
to reach only about 60% extraction efficiency [66].
2.4.2 MAE Versus Supercritical Fluid Extraction (SFE)
For green extraction, the use of SFE is very attractive because the solute is easily
recovered and the solvent can be recycled by the simple manipulation of parameters
such temperature and/or pressure. Supercritical fluids present liquid-like densities,
whereas their viscosity is near that of normal gases and their diffusivity is about two
orders of magnitude higher than in typical liquids [91]. Carbon dioxide (CO2) is the
most used solvent in SFE because it is safe, nontoxic, and generally available at a
reasonable cost. However, even at high densities, CO2 has a limited ability to dis-
solve highly polar compounds. The addition of modifiers to CO2 can improve the
extraction efficiency by increasing the solubility of the solute in the solvent.
The ease of tuning the operating conditions to increase the solvation power
makes this technology a good option for the selective recovery of several types of
substances. This combination of properties makes SFE an important process in the

food, pharmaceutical, and cosmetic industries because it is possible to fabricate
products without toxic residues, with no degradation of active principles, and with
high purity. Thus, SFE can be a fast, efficient, and clean method for the extraction
of natural products from vegetable matrices [92].
Compared to SFE, MAE has a disadvantage, because cleanup is usually needed
for this relatively selective technique [8, 63]. However, method development is often
more complex in SFE and additionally sample throughput is not as high as in MAE
[8]. Furthermore, the efficiency of MAE can be poor when either the target com-
pounds or solvents are nonpolar, or when they are volatile. According to Stalikas
[93], drying of the samples can be avoided for sample preparation with MAE,
whereas samples are usually dried before SFE.
From the economic point of view, MAE is feasible as it requires moderate cost
for equipment setup [63] and is much cheaper as compared to SFE. Moreover, MAE
has low risks and no major safety issues as most extractions are generally carried
out under atmospheric condition [28].
Several studies compared SFE and MAE. Hao et al. [66] extracted artemisinin
from Artemisia annua L. by MAE, Soxhlet, and SFE. They found that MAE saves
much time (12 min) and gives a high extraction rate (92.1%); SFE gives the lightest
extract color but the lowest extraction yield while several hours were needed for
Soxhlet. The same results were found by Grigonis et al. [64] comparing MAE with
SFE and Soxhlet. The MAE gave the most concentrated extract with 8.15% of
5,8-dihydroxycoumarin (extract yield, 0.42%) from sweet grass. In addition, only
5 min gave the highest yield of triterpenoid saponins (0.968%), whereas SFE and
UAE required several hours or even more than 10 h and gave a lower yield [40].
2.4.3 MAE Versus Ultrasound-Assisted Extraction (UAE)
Ultrasound-assisted extraction (UAE) in the food industry has been the subject of
research and development; its emergence as a green novel technology has also
attracted attention to its role in environmental sustainability [94]. Ultrasound has
been used in various processes of the chemical and food industries; it is a rapid
technique, consumes small amounts of fossil energy, and allows reducing solvent
consumption, thus resulting in a more pure product and higher yields.
The principle of high-power ultrasound has been attributed to the acoustic cavita-
tion phenomenon that appears when high-intensity acoustic waves are generated in
a fluid [95]. The extraction mechanism involves two types of physical phenomena:
diffusion through the cell walls and washing out the cell content once the walls are
broken [96]. Ultrasound waves modify their physical and chemical properties after
their interaction with subjected plant material, and their cavitational effects facili-
tate the release of extractable compounds and enhance mass transport by disrupting
the plant cell walls [94, 97, 98].
Developments in ultrasound technology and its potential benefits have triggered

interest in the application of power ultrasound on a wider range of chemistry
processing [99].
The combination of sonication and microwaves was studied for extraction of
lipids from vegetables and microalgae sources. Ultrasonication alone, microwave
irradiation alone, or a combination of both techniques gave excellent extraction
efficiencies in term of yield and time, with a tenfold reduction in the time needed
with conventional methods, and increase of yields from 50% to 500% [74]. MAE
possessed higher efficiency (11.62%) for the extraction of triterpene saponins from
yellow horn (Xanthoceras sorbifolia Bunge.) compared with UAE (6.78%) and
reflux extraction (10.82%) [43].
2.4.4 MAE Versus Pressurized Liquid Extraction (PLE)
Pressurized liquid extraction (PLE), also referred to as pressurized solvent extrac-

tion (PSE) and accelerated solvent extraction (ASE), is now well accepted as an
alternative to Soxhlet extraction [100] and has been successfully used to isolate
antioxidants from plants [101], such as thermolabile anthocyanins from jabuticaba
(Myrciaria cauliflora) [102].
The use of the PLE technique is an attractive alternative because it allows fast
extraction and reduced solvent consumption [102]. This technique allows the use of
solvents or solvent mixtures with different polarities under high pressures (up to
20 MPa), keeping the extraction solvent in the liquid state [103], and temperatures
ranging from room temperature up to 200°C [104].
The pressurized solvent at a determined temperature is pumped into an extrac-
tion vessel containing the sample matrix. Using high temperature accelerates the
extraction process by increasing the solubility of the analytes in the solvent and thus
increasing the kinetic rate of desorption of the solute from the sample matrix; this
occurs because the pressurized solvent remains in the liquid state well above its
boiling point, allowing high-temperature extraction [103]. Considerable increase in
the mass transfer rates results from the decrease of viscosity and superficial tension
of the solvent.
Moreover, the use of high temperatures, which on the one hand increases extrac-
tion rates, on the other hand may lead to degradation of thermolabile compounds
[105]. PLE uses liquid solvents; therefore, its basic principle is considered similar
to those of classic extraction. Partly because these newer technologies are auto-
mated and the solvents are under “superheated” conditions (the effect of micro-
waves in MAE or elevated temperature or pressure in PLE), they are more user
friendly, much quicker, and require significantly less organic solvent [49].
Although in PLE the filtration step is “included” in the process, in MAE a cleanup
step is often needed. MAE is considered an easy technique, and compared to SFE
and PLE, it is less expensive [8].
Although good recovery rates were obtained with both extraction methods,
MAE provided advantages with regard to sample handling, cost, analysis time, and
solvent consumption.
2.5 Conclusion
There has been much research and many advances in development in the microwave-
assisted extraction of a number of plant compounds. This chapter showed the
phenomena of mass and heat transfer of the MAE process as well the parameters
that influence MAE extraction of bioactive compounds. Therefore, optimized operat-
ing parameters can improve MAE performance. Also, MAE is better or comparable
with other techniques. As a concluding remark, the MAE system is considered a
promising technique for plant extraction because of its use of different physical and
chemical phenomena compared to those in conventional extractions.
Acknowledgments Priscilla C. Veggi thanks Fundação de Amparo a Pesquisa do Estado de

São Paulo (FAPESP) for Ph.D. assistantships (2008/10986-2). The authors thank FAPESP
(2009/17234-9) and CNPq (302778/2007-1) for financial support.
References
1. Chemat F, Abert-Vian M, Zill-e-Huma Y-J (2009) Microwave assisted separations: green

chemistry in action. In: Pearlman JT (ed) Green chemistry research trends. Nova Science
Publishers, New York, pp 33–62
2. Périno-Issartier S, Zill-e-Huma Y-J, Abert-Vian M, Chemat F (2011) Solvent free micro-
wave-assisted extraction of antioxidants from sea buckthorn (Hippophae rhamnoides) food
by-products. Food Bioprocess Technol 4:1020–1028
3. Aguilera JM (2003) Solid–liquid extraction. In: Tzia C, Liadakis G (eds) Extraction optimi-
zation in food engineering. Dekker, New York, pp 35–55
4. Hu Z, Cai M, Liang HH (2008) Desirability function approach for the optimization of micro-
wave-assisted extraction of saikosaponins from Radix bupleuri. Sep Purif Technol
61(3):266–275
5. Raynie DE (2000) Extraction. In: Wilson ID, Adlard ER, Cooke M, Poolie CF (eds)
Encyclopedia of separation science. Academic Press, San Diego
6. Majors RE (2008) Practical aspects of solvent extraction. LCGC N Am 26(12):1158–1166
7. Routray W, Orsat V (2011) Microwave-assisted extraction of flavonoids: a review. Food
Bioprocess Technol 5(2):1–16
8. Eskilsson CS, Björklund E (2000) Analytical-scale microwave-assisted extraction. J Chromatogr
A 902:227–250
9. Thostenson ET, Chou TW (1999) Microwave processing: fundamentals and applications.
Compos Part A Appl S 30(9):1055–1071
10. Metaxas AC, Meredith RJ (1983) Industrial microwave heating. Peter Peregrinus, London,
pp 28–31
11. Kingston HM, Jassie LB (1988) Introduction to microwave sample preparation. American
Chemical Society, Washington, DC
12. Acierno D, Barba AA, d’Amore M (2004) Heat transfer phenomena during processing mate-
rials with microwave energy. Heat Mass Transfer 40:413–420
13. Mandal V, Mohan Y, Hemalath S (2007) Microwave assisted extraction-an innovative and
promising extraction tool for medicinal plant research. Phcog Rev 1(1):7–18
14. Jassie L, Revesz R, Kierstead T, Hasty E, Metz S (1997) In: Kingston HM, Haswell SJ (eds)
Microwave-enhanced chemistry. American Chemical Society, Washington, DC, p 569
15. Zlotorzynski A (1995) The application of microwave radiation to analytical and environmental
chemistry. Crit Rev Anal Chem 25:43–75
16. Jain T, Jain V, Pandey R, Vyas A, Shukla SS (2009) Microwave assisted extraction for phy-
toconstituents: an overview. Asian J Res Chem 2(1):19–25
17. Buffler CR (1993) Microwave cooking and processing: engineering fundamentals for the
food scientist. Van Nostrand Reinhold, New York
18. Chen M, Siochi EJ, Ward TC, McGrath JE (1993) Basic ideas of microwave processing of
polymers. Polym Eng Sci 33:1092–1109
19. Abhayawick L, Laguerre JC, Tauzin V, Duquenoy A (2002) Physical properties of three
onion varieties as affected by the moisture content. J Food Eng 55:253–262
20. Al-Harahshed M, Kingman SW (2004) Microwave-assisted leaching: a review.
Hydrometallurgy 73:189–203
21. Datta AK (2007) Porous media approaches to studying simultaneous heat and mass transfer
in food processes. I: Problem formulations. J Food Eng 80:80–95
22. Datta AK (2007) Porous media approaches to studying simultaneous heat and mass transfer
in food processes. II: Property data and representative results. J Food Eng 80:96–110
23. Takeuchi TM, Pereira CG, Braga MEM, Maróstica MR Jr, Leal PF, Meireles MAA (2009)
Low-pressure solvent extraction (solid–liquid extraction, microwave-assisted, and ultra-
sound-assisted) from condimentary plants. In: de Almeida Meireles MA (ed) Extracting bio-
active compounds for food products, 1st edn. CRC Press/Taylor & Francis, Boca Raton, pp
137–218
24. Navarrete A, Mato RB, Cocero MJ (2012) A predictive approach in modeling and simulation
of heat and mass transfer during microwave heating. Application to SFME of essential oil of
lavandin super. Chem Eng Sci 68:192–201
25. Sihvola A (2000) Mixing rules with complex dielectric coefficients. Subsurf Sensing Technol
Appl 1:393–415
26. Chen L, Song D, Tian Y, Ding L, Yu A, Zhang H (2008) Application of on-line microwave
sample-preparation techniques. Trends Anal Chem 27:151–159
27. Spigno G, De Faveri DM (2009) Microwave-assisted extraction of tea phenols: a phenomeno-
logical study. J Food Eng 93:210–217
28. Chan C-H, Yusoff R, Ngoh G-C, Kung FW-L (2011) Microwave-assisted extractions of
active ingredients from plants. J Chromatogr A 1218:6213–6225
29. Tatke P, Jaiswal Y (2011) An overview of microwave assisted extraction and its applications
in herbal drug research. Res J Med Plants 5:21–31
30. Brachet A, Christen P, Veuthey JL (2002) Focused microwave-assisted extraction of cocaine
and benzoylecgonine from coca leaves. Phytochem Anal 13:162–169
31. Wang L, Weller CL (2006) Recent advances in extraction of nutraceuticals from plants.
Trends Food Sci Technol 17:300–312
32. Zhou H-Y, Liu C-Z (2006) Microwave-assisted extraction of solanesol from tobacco leaves.
J Chromatogr A 1129:135–139
33. Zigoneanu IG, Williams L, Xu Z, Sabliov CM (2008) Determination of antioxidant compo-
nents in rice bran oil extracted by microwave-assisted method. Bioresour Technol
99:4910–4918
34. Talebi M, Ghassempour A, Talebpour Z, Rassouli A, Dolatyari L (2004) Optimization of the
extraction of paclitaxel from Taxus baccata L. by the use of microwave energy. J Sep Sci
27:1130–1136
35. Song J, Li D, Liu C, Zhang Y (2011) Optimized microwave-assisted extraction of total phe-
nolics (TP) from Ipomoea batatas leaves and its antioxidant activity. Innov Food Sci Emerg
Technol 12:282–287
36. Pan X, Niu G, Liu H (2003) Microwave assisted extraction of tea polyphenols and tea caffeine
from green tea leaves. Chem Eng Process 42:129–133
37. Eskilsson CS, Björklund E, Mathiasson L, Karlsson L, Torstensson A (1999) Microwave-
assisted extraction of felodipine tablets. J Chromatogr A 840:59–70
38. Llompart MP, Lorenzo RA, Cela R, Jocelyn Pare JR, Belanger JMR, Li K (1997) Phenol and
methylphenol isomers determination in soils by in-situ microwave-assisted extraction and
derivatisation. J Chromatogr A 757:153–164
39. Lu Y, Ma W, Hu R, Dai X, Pan Y (2008) Ionic liquid-based microwave-assisted extraction of phe-
nolic alkaloids from the medicinal plant Nelumbo nucifera Gaertn. J Chromatogr A 1208:42–46
40. Chen Y, Xie M-Y, Gong X-F (2007) Microwave-assisted extraction used for the isolation of
total triterpenoid saponins from Ganoderma atrum. J Food Eng 81:162–170
41. Wang Y, You J, Yu Y, Qu C, Zhang H, Ding L et al (2008) Analysis of ginsenosides in Panax
ginseng in high pressure microwave-assisted extraction. Food Chem 110(1):161–167
42. Xiao W, Han L, Shi B (2008) Microwave-assisted extraction of flavonoids from Radix astra-
gali. Sep Purif Technol 62(3):614–618
43. Li J, Zu Y-G, Fu Y-J, Yang Y-C, Li S-M, Li Z-N, Wink M (2010) Optimization of microwave-
assisted extraction of triterpene saponins from defatted residue of yellow horn (Xanthoceras
sorbifolia Bunge.) kernel and evaluation of its antioxidant activity. Innov Food Sci Emerg
Technol 11:637–664
44. Yan MM, Liu W, Fu YJ, Zu YG, Chen CY, Luo M (2010) Optimisation of the microwave-
assisted extraction process for four main astragalosides in Radix astragali. Food Chem
119(4):1663–1670
45. Chemat S, Ait-Amar H, Lagha A, Esveld DC (2005) Microwave-assisted extraction kinetics
of terpenes from caraway seeds. Chem Eng Process 44:1320–1326
46. Khajeh M, Akbari Moghaddam AR, Sanchooli E (2009) Application of Doehlert design in
the optimization of microwave assisted extraction for determination of zinc and copper in
cereal samples using FAAS. Food Anal Methods 3(3):133–137
47. Alfaro MJ, Belanger JMR, Padilla FC, Pare JRJ (2003) Influence of solvent, matrix dielectric
properties, and applied power on the liquid-phase microwave-assisted processes (MAP™)1
extraction of ginger (Zingiber officinale). Food Res Int 36:499–504
48. Raner KD, Strauss CR, Vyskoc F, Mokbel L (1993) A comparison of reaction kinetics
observed under microwave irradiation and conventional heating. J Org Chem 58:950–995
49. Huie CW (2002) A review of modern sample-preparation techniques for the extraction and
analysis of medicinal plants. Anal Bioanal Chem 373:23–30
50. Ruan GH, Li GKJ (2007) The study on the chromatographic fingerprint of Fructus xanthii by
microwave assisted extraction coupled with GC-MS. J Chromatogr B 850:241–248
51. Kovács Á, Ganzler K, Simon-Sarkadi L (1998) Microwave-assisted extraction of free amino
acids from foods. Z Lebensm Unters Forsch A 207:26–30
52. Michel T, Destandau E, Elfakir C (2011) Evaluation of a simple and promising method for
extraction of antioxidants from sea buckthorn (Hippophaë rhamnoides L.) berries: pres-
surised solvent-free microwave-assisted extraction. Food Chem 126:1380–1386
53. Fan JP, Zhang RF, Zhu JH (2010) Optimization of microwave-assisted extraction of total
triterpenoid in Diospyros kaki leaves using response surface methodology. Asian J Chem
22(5):3487–3500
54. Nyiredy S (2004) Separation strategies of plant constituents: current status. J Chromatogr B
812:35–51
55. Yuan L, Li H, Ma R, Xu X, Zhao C, Wang Z, Chen F, Hu X (2012) Effect of energy density
and citric acid concentration on anthocyanins yield and solution temperature of grape peel in
microwave-assisted extraction process. J Food Eng 109:274–280
56. Dhobi M, Mandal V, Hemalatha S (2009) Optimization of microwave assisted extraction of
bioactive flavonolignan–silybinin. J Chem Metrl 3(1):13–23
57. Chemat F, Smadja J (2004) Brevet Européen. EP 1 439 218 A1
58. Vian M, Fernandez X, Visinoni F, Chemat F (2008) Solvent free microwave extraction of
Elletaria cardamomum L.: a multivariate study of a new technique for the extraction of essen-
tial oil. J Chromatogr A 1190:14–17
59. Mengal P, Mompon B (1996) Method and apparatus for solvent free microwave extraction of
natural products. Eur Patent P EP 698,076 B1
60. Virot M, Tomao V, Colnagui G, Visinoni F, Chemat F (2007) New microwave-integrated
Soxhlet extraction. An advantageous tool for the extraction of lipids from food products.
J Chromatogr A 1174:138–144
61. Chemat F, Smadja J, Lucchesi ME (2004) Solvent-free microwave extraction of volatile natu-
ral substances. US Patent 0,187,340, A1
62. Clayton B (1999) Heating with microwaves, Engineering World, 4–6
63. Wang LJ (2010) Advances in extraction of plant products in nutraceutical processing. In:
Pathak Y (ed) Handbook of nutraceuticals, vol II: Scale up, processing and automation. CRC
Press/Taylor & Francis, Boca Raton, pp 15–52
64. Chemat F, Abert-Vian M, Visinoni F (2008) Microwave hydrodiffusion for isolation of natu-
ral products. European Patent EP 1,955,749 A1
65. Grigonis D, Venskutonis PR, Sivik B, Sandahl M, Eskilsson CS (2005) Comparison of differ-
ent extraction techniques for isolation of antioxidants from sweet grass (Hierchloë odorata).
J Supercrit Fluids 33:223–233
66. Hao J-Y, Han W, Huang S-D, Xue B-Y, Deng X (2002) Microwave-assisted extraction of
artemisinin from Artemisia annua L. Sep Purif Technol 28(3):191–196
67. Pan X, Liu H, Jia G, Shu YY (2000) Microwave-assisted extraction of glycyrrhizic acid from
licorice root. Biochem Eng J 5:173–177
68. Bagherian H, Ashtiani FZ, Fouladitajar A, Mohtashamy M (2011) Comparisons between
conventional, microwave- and ultrasound-assisted methods for extraction of pectin from
grapefruit. Chem Eng Process 50:1237–1243
69. Chen Y, Ming-Yong X, Xiao-Feng G (2007) Microwave-assisted extraction used for the iso-
lation of total triterpenoid saponins from Ganoderma atrum. J Food Eng 81:162–170
70. Wakte PS, Sachin BS, Patil AA, Mohato DM, Band TH, Shinde DB (2011) Optimization of
microwave, ultrasonic and supercritical carbon dioxide assisted extraction techniques for cur-
cumin from Curcuma longa. Sep Purif Technol 79:50–55
71. Gallo M, Ferracane R, Graziani G, Ritieni A, Fogliano V (2010) Microwave assisted extrac-
tion of phenolic compounds from four different spices. Molecules 15:6365–6374
72. Raghavan S, Richards MP (2007) Comparison of solvent and microwave extracts of cran-
berry press cake on the inhibition of lipid oxidation in mechanically separated turkey. Food
Chem 102(3):818–826
73. Hemwimon S, Pavasant P, Shotipruk A (2007) Microwave-assisted extraction of antioxida-
tive anthraquinones from roots of Morinda citrifolia. Sep Purif Technol 54(1):44–50
74. Cravotto G, Boffa L, Mantegna S, Perego P, Avogadro M, Cint P (2008) Improved extraction
of vegetable oils under high-intensity ultrasound and/or microwaves. Ultrason Sonochem
15(5):898–902
75. Chemat F, Lucchesi ME, Smadja J, Favretto L, Colnaghi G, Visinoni F (2006) Microwave
accelerated steam distillation of essential oil from lavender: a rapid, clean and environmen-
tally friendly approach. Anal Chim Acta 555(1):157–160
76. Farhat A, Fabiano-Tixier A-S, Visinoni F, Romdhane M, Chemat F (2010) A surprising
method for green extraction of essential oil from dry spices: microwave dry-diffusion and
gravity. J Chromatogr A 1217(47):7345–7350
77. Hongyan L, Deng Z, Wu T, Liu R, Loewen S, Tsao R (2012) Microwave-assisted extraction
of phenolics with maximal antioxidant activities in tomatoes. Food Chem 130(4):928–936
78. Kapás Á, András CD, Dobre TG, Székly G, Stroescu M, Lányi S, Ábrahám B (2011) The
kinetic of essential oil separation from fennel by microwave assisted hydrodistillation
(MWHD). UPB Sci Bull Ser B 73(4):113–120
79. Kaufmann B, Christen P, Jean-Luc V (2001) Parameters affecting microwave-assisted extrac-
tion of withanolides. Phytochem Anal 12(5):327–331
80. Lucchesi ME, Chemat F, Smadja J (2004) Solvent-free microwave extraction of essential
oil from aromatic herbs: comparison with conventional hydro-distillation. J Chromatogr A
1043(2):323–327
81. Lucchesi ME, Smadja J, Bradshaw S, Louw W, Chemat F (2007) Solvent free microwave
extraction of Elletaria cardamomum L.: a multivariate study of a new technique for the
extraction of essential oil. J Food Eng 79(3):1079–1086
82. Mandal V, Dewanjee S, Mandal SC (2009) Microwave-assisted extraction of total bioactive
saponin fraction from Gymnema sylvestre with reference to gymnemagenin: a potential bio-
marker. Phytochem Anal 20(6):491–497
83. Martino E, Ramaiola I, Urbano M, Bracco F, Collina S (2006) Microwave-assisted extraction
of coumarin and related compounds from Melilotus officinalis (L.) Pallas as an alternative to
Soxhlet and ultrasound-assisted extraction. J Chromatogr A 1125(2):147–151
84. Pan X, Niu G, Liu H (2001) Microwave-assisted extraction of tanshinones from Salvia milti-
orrhiza Bunge. with analysis by high-performance liquid chromatography. J Chromatogr A
922(1–2):371–375
85. Sahraoui N, Vian MA, Bornard I, Boutekedjiret C, Chemat F (2008) Improved microwave
steam distillation apparatus for isolation of essential oils: comparison with conventional
steam distillation. J Chromatogr A 1210(2):229–233
86. Zill-e-Huma Y-J, Vian MA, Fabiano-Tixier A-S, Elmaataoui M, Dangles O, Chemat F (2011)
A remarkable influence of microwave extraction: enhancement of antioxidant activity of
extracted onion varieties. Food Chem 127(4):1472–1480
87. Jensen WB (2007) The origin of the Soxhlet extractor. J Chem Educ 84(12):1913–1914
88. de Luque Castro MD, Garcia-Ayuso LE (1998) Soxhlet extraction of solid materials: an out-
dated technique with a promising innovative future. Anal Chim Acta 369:1–10
89. Kaufmann B, Christen P, Veuthey J-L (2001) Parameters affecting microwave-assisted extrac-
tion of withanolides. Phytochem Anal 12:327–331
90. Pan X, Niu G, Liu H (2002) Comparison of microwave-assisted extraction and conventional
extraction techniques for the extraction of tanshinones from Salvia miltiorrhiza Bunge.
Biochem Eng J 12:71–77
91. Brunner G (2005) Supercritical fluids: technology and application to food processing. J Food
Eng 67:21–33
92. Pereira CG, Meireles MAA (2010) Supercritical fluid extraction of bioactive compounds: fun-
damentals, applications and economic perspectives. Food Bioprocess Technol 3:340–372
93. Stalikas CD (2007) Extraction, separation, and detection methods for phenolic acids and
flavonoids. J Sep Sci 30(18):3268–3295
94. Chemat F, Zill-e-Huma Y-J, Khan MK (2011) Applications of ultrasound in food technology:
processing, preservation and extraction. Ultrason Sonochem 18(4):813–835
95. Jian-bing J, Xiang-hong L, Mei-qiang C, Zhi-chao X (2006) Improvement of leaching pro-
cess of geniposide with ultrasound. Ultrason Sonochem 13(5):455–462
96. Gaete-Garretón L, Vargas-Hernández Y, Cares-Pacheco MG, Sainz J, Alarcón J (2011)
Ultrasonically enhanced extraction of bioactive principles from Quillaja saponaria Molina.
Ultrasonics 51(5):581–585
97. Mason TJ, Paniwnyk L, Lorimer JP (1996) The use of ultrasound in food technology. Ultrason
Sonochem 3(3):253–8260
98. Vinatoru M (2001) Na overview of the ultrasonically assisted extraction of bioactive princi-
ples from herns. Ultrason Sonochem 8(3):303–313
99. Sivakumar V, Ravi Verma V, Rao PG, Swaminathan G (2007) Studies on the use of power
ultrasound in solid–liquid myrobalan extraction process. J Cleaner Prod 15(18):1815–1820
100. Majors RE (2006) Modern techniques for the extraction of solid materials: an update. LC-GC
N Am 24(7):648–660
101. Cha KH, Kang SW, Kim CY, Um BH, Na YR, Pan CH (2010) Effect of pressurized liquids
on extraction of antioxidants from Chlorella vulgaris. J Agric Food Chem 58(8):4756–4761
102. Santos DT, Veggi PC, Meireles MAA (2012) Optimization and economic evaluation of pres-
surized liquid extraction of phenolic compounds from jabuticaba skins. J Food Eng
108:444–452
103. Richter BE, Jones BA, Ezzell JL, Porter NL (1997) Accelerated solvent extraction: a new
technique for sample preparation. Anal Chem 68(6):1033–1039
104. Kaufmann B, Christen P (2002) Recent extraction techniques for natural products: micro-
wave-assisted extraction and pressurised solvent extraction. Phytochem Anal
13(2):105–113
105. Brachet A, Rudaz S, Mateus L, Christen P, Veuthey J-L (2001) Optimisation of accelerated
solvent extraction of cocaine and benzoylecgonine from coca leaves. J Sep Sci
24(10–11):865–873
http://www.springer.com/978-1-4614-4829-7

Uploaded by

Copyright:

Available Formats

Uploaded by

Copyright:

Available Formats

Chapter 2

Fundamentals of Microwave Extraction

Priscilla C. Veggi, Julian Martinez, and M. Angela A. Meireles

2.1 Basic Principles

2.1.1 Mechanism of Microwave Extraction

P.C. Veggi (*) • J. Martinez • M.A.A. Meireles

F. Chemat and G. Cravotto (eds.), Microwave-assisted Extraction for Bioactive 15

2.1.2 Mechanism of Microwave Heating

In the microwave heating process, energy transfer occurs by two mechanisms:

2.1.3 Heat Transfer in Microwave Heating

T(x, y, z, t) t = 0 = T0 (x, y, z ) (2.4)

The convective boundary condition at the material surfaces is given by Newton’s

where n is the specific dimension, a is the boundary position, h is the convective

where P is the microwave power dissipation per volume unit, K is a constant, f

where l0 is the wavelength in vacuum and d the approximate penetration depth.

2.2 Heat and Mass Transfer: Balance Equations and Kinetics

Plant materials can be considered as porous media because of their similarities to

2.2.1 Heat and Mass Balance Equations for Solid–Liquid MAE

Diffusion coefficient data are necessary to make calculations. Diffusivities may

If pure solvent is used initially, CC0 = 0, and then

2.2.2 Heat and Mass Balance Equations for SFMAE

where w is the angular frequency of the electromagnetic wave, eo is the vacuum

CP = rS CPS (1 − j )+ rw CPwj Sw + rg CPgj (1 − Sw ) (2.22)

where M w is the plant material moisture, which is calculated from

where r B is the bed apparent density.

2.3 Important Parameters in Microwave-Assisted

The optimization of MAE conditions has been studied in several applications.

2.3.1 Effect of Solvent System and Solvent-to-Feed Ratio (S/F)

2.3.2 Effect of Extraction Time and Cycle

In MAE the period of heating is another important factor to be considered. Extraction

2.3.3 Effect of Microwave Power and Extraction Temperature

2.3.4 Effect of Contact Surface Area and Water Content

2.3.5 Effect of Stirring

2.4 Comparison of Microwave-Assisted Extraction (MAE) with

To introduce bioactive plant extracts in pharmaceutical and cosmetic formulations,

The ideal extraction technology depends on the type of compound to be extracted,

s = ethanol; S/F = 10; t = 10 h

Plant material (P/F), humidity (h) basis, wb) References

s = water; S/F = 30; T = 70 C; t = 25 min

s = ethanol (9.5: 0.5 v/v); S/F = 25; T = 95 C; t = 1 h

Operational conditions: type of solvent(s), solvent to feed ratio (S/F),

Maceration: Silybinin (0.36% dba)

Cuminum cyminum MAE: Phenolics content (1.159% dbb) [71]

Operational conditions: type of solvent(s), solvent to feed ratio (S/F),

SD: Monoterpenes (4.92% dba)

Table 2.3 (continued)

Global yield (0.028% wba)

Mentha crispa L. (garden SFME: Limonene (9.7% wba) [80]

L. Pw = 390 W; T = 100 C; h = 67%; t = 75 min

s = methanol: water (85: 15 v/v); S/F = 100; t = 24 h

Operational conditions: type of solvent(s), solvent to feed ratio (S/F),

Astragaloside IV (0.257% dba)

Table 2.3 (continued)

2.4.1 MAE Versus Soxhlet

2.4.2 MAE Versus Supercritical Fluid Extraction (SFE)

substances. This combination of properties makes SFE an important process in the

2.4.3 MAE Versus Ultrasound-Assisted Extraction (UAE)

Developments in ultrasound technology and its potential benefits have triggered

2.4.4 MAE Versus Pressurized Liquid Extraction (PLE)

Pressurized liquid extraction (PLE), also referred to as pressurized solvent extrac-

Acknowledgments Priscilla C. Veggi thanks Fundação de Amparo a Pesquisa do Estado de

1. Chemat F, Abert-Vian M, Zill-e-Huma Y-J (2009) Microwave assisted separations: green

You might also like