Microwave Assisted Water Extraction of Plant Compounds

Review
Received: 20 June 2014
Revised: 12 August 2014
Accepted article published: 19 August 2014
Published online in Wiley Online Library: 22 September 2014
(wileyonlinelibrary.com) DOI 10.1002/jctb.4519
Microwave assisted water extraction

of plant compounds
Noelia Flrez, Enma Conde and Herminia Domnguez*
Abstract
The development of environmentally friendly processes with limited generation of polluting streams to attain sustainable
utilization of raw materials is encouraged. The implementation of novel extraction technologies more ecient, selective and
with lower energy consumption than conventional ones, can help in achieving this objective. Particularly promising are aqueous
based methods, since water is a cheap, safe and abundant solvent and the limited use of toxic organic solvents is a consumer s,
ecological and processing demand. The benets and the limiting aspects of microwave assisted water extraction, either adding
water as the only solvent or in solvent free processes, using the naturally present water in vegetal materials for the extraction
of valuable components from renewable vegetal sources are highlighted and the potential of this technique for industrial
applications is discussed.
2014 Society of Chemical Industry
Keywords: microwave; solidliquid extraction; water; solvent free; plant compounds
INTRODUCTION
590
Recent trends in chemical design of manufacturing processes have

been focused on limiting the damage to the environment, providing sustainable alternatives that maximize the ecient use
of materials and reduce the waste produced. The importance of
green chemistry has been particularly evidenced in some industries, such as food, cosmetics, nutraceuticals and pharmaceuticals
in order to develop safer products.
Solidliquid extraction is a unit operation essential for isolation
of natural plant compounds and proper optimization is required to
reduce the energy consumption of the whole process.1 The bottlenecks that traditional solvent extraction technologies should
overcome include reduction of energy consumption and fulllment of increasingly stringent legal requirements on emissions
and safety and control of materials, processes and products. Some
alternative techniques reduce solvent consumption and extraction time and are suited for thermolabile constituents enabling
cost-eective production of high quality extracts. Among these
green technologies it is relatively easy to scale up extraction
assisted by ultrasound, by microwaves and extraction with pressurized liquids.2,3 Microwave assisted extraction is based on heating the solvent by application of microwave energy. Excellent
overviews are found on microwave reaction chemistry, including
the principles of microwave dielectric heating, instrumentation,
and applications,4 potential for organic reactions5 and combination with water as solvent for organic transformations,6 8 into
drugs and ne chemicals.9 Microwave applications in processing and preservation of food materials10 and sample preparation
are available.11,12 Comprehensive recent reviews on the extraction of natural compounds and secondary plant metabolites with
bioactive properties13 19 and pharmaceutical and nutraceutical
applications20 have been published.
The relevance and potential of water under pressurized conditions for solidliquid extraction aided by ultrasound and
J Chem Technol Biotechnol 2015; 90: 590607
microwaves was critically reviewed.21 In the last decade a number

of studies have proposed water as the only solvent or in solvent
free microwave assisted processes for the extraction of plant
compounds. In the present review information on this subject
is updated and the potential of water as a green solvent for
microwave assisted technology is examined and illustrated with
examples.
WATER AS A GREEN EXTRACTION SOLVENT

Solvents are widely used in commercial manufacturing and service
industries as processing aids, cleaning agents and dispersants. The
selection of the solvent is critical in designing optimal extraction
operations, since it has economical, environmental and social
implications, because solvents are dicult to contain and recycle
and can contaminate air, land, and water. Replacement of hazardous, toxic, volatile and highly ammable solvents with other
showing superior ecological, health and safety properties or with
green solvents produced from renewable resources is a priority
in green chemistry,7,9,22 and the use of GRAS (general recognize
as safe) solvents is incentivized. The search for environmentally
benign solvent alternatives has led to the reduction of solvent
use and/or to more ecient recycling protocols to limit industrial
emissions and, where appropriate, to solvent free processes.
To reach the full potential of alternative solvents, their intrinsic
environmental advantages and those related to performance, solubility, inertness, health, cost, and safety should be considered.23
Correspondence to: H. Domnguez, Departamento de Enxeera Qumica, Universidade de Vigo (Campus Ourense), Edicio Politcnico, As Lagoas, 32004
Ourense, Spain. E-mail: herminia@uvigo.es
Departamento de Enxeera Qumica, Universidade de Vigo (Campus Ourense),
Edicio Politcnico, As Lagoas, 32004 Ourense, Spain
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Microwave assisted water extraction of plant compounds
Figure 1. Eect of temperature on: (a) the dielectric constant and density of
water compared with values for conventional solvents in the same range of
temperatures of the liquid state; and (b) the water solubility of some model
compounds.
water was initially used to extract contaminants from soils and

other matrices; more recently it has been proposed to extract
bioactives from plants, and as a solvent for biomass conversion
since it is an excellent medium for fast, homogeneous and ecient
reactions, attractive from the viewpoint of energy consumption,
process integration32 and scale up.33
The traditional distillation for removing solvent from product
is expensive, time-consuming, and when water is used as solvent its green quality could be overlooked since water-based processes are usually very energy intensive to concentrate the extract.
Among the alternatives, addition of a solvent to precipitate the
product does not replace distillation, but membrane-based processes are more promising.34 Membranes have also been used to
fractionate and concentrate the diluted aqueous extracts obtained
with hot water at atmospheric conditions32 and with pressurized
hot water.35 37
FUNDAMENTALS OF MICROWAVE HEATING

Microwaves (MW) are radiation of the electromagnetic spectrum
ranging in frequency from 300 MHz (radio radiation) to 300 GHz
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591
Finding and recognizing a green solvent, an easily-removable

polar aprotic solvent and eliminating distillation are among the
major challenges that could decrease the environmental impact of
solvents. Those solvents that would provide the greatest reduction
in environmental damage are CO2 , water, and carefully selected
traditional organic solvents.24
Water seems the greenest solvent, being nontoxic, noncorrosive, non-ammable, environmentally benign, naturally
abundant, and available at low cost. However, water has some
limitations to being converted to a universal sustainable alternative for solvent extraction processes,25 such as the low solubility of
apolar compounds and the energetic requirements to concentrate
products.
The extraction of apolar compounds requires apolar or semipolar solvents, which are often toxic and should be removed if
the extract is destined for food or pharmaceutical applications.
Volatile organic solvents are usually ammable, contribute to
smog formation and present health risks. One alternative could
be subcritical water (SCW). Water exists in the supercritical state
at temperatures above 374 C and pressures above 221 bar. Subcritical or near-critical water, in the range between 100 C and the
critical temperature, also named as pressurized low polarity water,
pressurized hot water, superheated water or high-temperature
water, shows advantages with regard to extraction eciency and
selectivity derived from the tunable polarity with temperature
and pressure.26 The polarity of water, measured by the dielectric
constant (Fig. 1(a)), decreases with increasing temperature. Above
100 C, the increased thermal agitation reduces the strength of
hydrogen bonds, leading to dielectric constant values similar to
those of organic solvents. Subcritical water can dissolve non-polar
compounds, whereas salts are less soluble.9,14,23 However, the
insolubility of hydrophobic materials in water when cooled to
room temperature makes the recovery of products dicult. The
solubility in SCW is dependent upon the structure of the solute
and substituents, i.e. benzoic acids showed an increase of about
two orders of magnitude,27 terpenes 25 to 6028 in the range
25200 C, and sugars even higher increases (Fig. 1(b)). Higher
temperatures in SCW extraction typically lead to rapid extraction
but degradation can occur, since the extracts are more prone to
undergo hydrolysis, oxidation, methylation, isomerization and
other reactions.26 Hydrolysis of plant materials may facilitate
extraction, but if the degraded extract is used as a foodstu or a
nutraceutical/pharmaceutical, caution regarding potential toxicity
of the products is required. The eciency of SCW depends on
the nature of the sample, the chemical structure of solute and
the extraction conditions. Pressure, usually kept high enough to
maintain water in the liquid phase, has a negligible eect on the
dielectric constant at pressure below 1000 bar and temperature is
the main parameter aecting extraction eciency and selectivity.
The enhanced extraction rates and yields in subcritical water
can be related to: (i) higher temperatures than in other extraction
techniques; (ii) improved solutesolvent contact due to lower
viscosity and surface tension, a relatively high density, in the range
between those of ambient and supercritical conditions, and high
solubility of organic substances; and (iii) hydrolytic reactions, that
break the cell walls facilitating the release of target compounds.26
The ionic product of subcritical water is relatively high (1012
compared with 1014 at ambient conditions), accelerating acidor base-catalyzed reactions. However, acidic and oxidizing media
can cause rapid corrosion, even more severe at subcritical than at
supercritical state.31 Therefore special materials and careful design
considering precipitation of inorganics are required. Subcritical
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(infrared radiation), which correspond with wavelengths from 1 m

to 1 mm. Household microwave ovens operate at 2450 MHz with
adjustable power output up to a maximum of 9001000 W.38,39
The MW energy, ranging from 1.24 106 to 1.24 103 eV, acts as
a nonionizing radiation that does not aect molecular structure
since it is lower than the usual ionization energies of biological
compounds (13.6 eV), bond energies (25 eV) and van der Waals
intermolecular interactions (<2 eV).40,41 The eect of MW on chemical synthesis and extraction processes is strictly related to the conversion of electromagnetic energy to heat;42,43 in controlled systems, high radiation intensity failed to show any other signicant
athermal or specic eects induced by microwave radiation.40,44
The principle of heating using microwave energy is based on the
direct eect of microwaves on molecules by dipole polarization
and ionic conduction.8 Owing to their electromagnetic nature,
microwaves possess electric eld and magnetic eld components
perpendicular to each other, and the concerted forces applied by
these components are rapidly changing in direction (2.4 109 per
second). Dipolar rotation is due to the alignment on the electric
eld of molecules possessing a dipole moment. The generation
of a phase dierence between the orientation of the eld and
that of the dipole produces molecular friction and collisions and
the liberation of thermal energy into the medium results in fast
dielectric heating.4,8,45 In liquids the ability of molecules to align
with the applied electric eld varies with frequency and with the
viscosity of the liquid. Conduction is the second major interaction
mechanism of the electric eld component with the sample. This
phenomena is responsible for the more rapid heating and higher
temperature reached in a solution containing ions than in another
without ions.8
The ability of a material to interact with electromagnetic energy
can be measured by the relative permitivity, a dimensionless complex value expressed as = j , where j is the imaginary unit.
The real component, , or dielectric constant is proportional to
the amount of energy absorbed. Compounds with large permanent dipole moments also have large dielectric constants, because
the dielectric polarization depends primarily on the ability of their
dipoles to reorientate in an electric eld.8,45 The imaginary component, , is the dielectric loss or loss factor and indicates the
ability of a medium to dissipate input dielectric energy as heat. The
eciency of microwave heating at a given frequency and temperature depends on the ability of the material to absorb electromagnetic energy and to dissipate heat, and can be measured by tan
= / , which is the energy dissipation factor or dielectric loss
tangent.
The dielectric properties dene the response of a given material
to electromagnetic waves; data for water and aqueous solutions
are well documented and interpreted45 but data for vegetal
matrices are scarce and greatly aected by the water content,
which can vary during processing.46 Water has higher dielectric
constant (80.4, value at ambient temperature and 2.45 GHz) but
low dielectric loss (0.123) than other conventional solvents such
as ethanol ( = 25.7, tan = 0.941), methanol ( = 32.7, tan
= 0.659) or acetone (= 20.6, tan = 0.054), determining that
the rate of microwave energy absorption by water is higher than
the dispersion of this energy into heat.47,48 Solvents with a high
dielectric constant and a high dissipation factor facilitate distribution of heat throughout the matrix and increase the extraction
yield of solutes. Non-polar solvents, which remain transparent
to microwaves due to their low dielectric constant and dissipation factor, are not heated under microwave irradiation,16 but
the addition of small amounts of a polar solvent with a large
N Flrez, E Conde, H Domnguez

loss tangent or the addition of salts usually enhances heating
rates.8,49
The conversion of microwave energy into heat can be calculated
as P = K f E2 tan , where P is the power dissipation (W cm3 ),
K is a constant (0.556 1010 ), f is the frequency applied (Hz),
is the absolute dielectric constant of the material, E is the electric
eld strength (V cm1 ), and tan is the dielectric loss tangent.
Dielectric heating rates also depend on the size, geometry and
quantity of the mixture and on the heat capacity of the medium.
The penetration depth, Dp , useful for scaling up purposes, is
dened as the distance from the surface at which the power
density has decreased to 1/e of its initial value at the surface.10,48
The penetration depth is much lower than the thickness of the
material, varies inversely with the loss factor and depends on the
frequency and dielectric properties of the material.
MECHANISM OF MICROWAVE ASSISTED

WATER EXTRACTION OF PLANT COMPONENTS
Understanding the cellular and subcellular localization of plant
metabolites is essential to study their extraction. Plant cells are
structures containing vacuoles and other organelles in the cytoplasm surrounded by a rigid wall, which consists of a framework of
cellulose microbrils embedded in a hydrophilic matrix of pectins
and hemicelluloses. The walls of adjacent cells are connected by
an amorphous pectin layer, the middle lamella. Other primary
metabolites of interest as solutes are: lipids, found in intracellular vacuoles (spherosomes) and proteins, accumulated both in
the storage vacuoles of dierentiated cells of the embryo and
endosperm and in protein bodies assembled within the endoplasmic reticulum.50 Phenolics are secondary metabolites that accumulate in cell vacuoles or can be ester or ether linked to cell wall
components, and essential oils are mostly present in special glands
named trichomes.
Extraction of solutes from plant materials is a mass transfer
process involving: (i) penetration of the solvent into the solid;
(ii) solubilizationdesorption of the solute from the solid matrix
and/or hydrolysis; (iii) diusion to the surface; and (iv) external
transfer into the bulk solution (Fig. 2). In solvent free systems the
rst step does not occur. Stages (i) and (iii) are diusion controlled
processes, slower than those based on equilibrium, reaction and
convective transport.
Disruption of the plant cells renders the protoplasm more permeable and is a crucial step in solidliquid extraction. Particle size
reduction by milling and grinding destroys cell integrity, reducing inner mass transfer limitations and facilitating the access of
the solvent to plant metabolites located in the cell walls or in the
cytoplasm. When water is used as the extracting solvent, viscosity and interfacial surface tension are reduced at high temperature, favouring the diusion of solvent through the solid matrix
and the solubility, whereas desorption of solutes from the matrix is
enhanced with the increased vapor pressure at elevated temperature. The elution of the extract solution that must diuse through
the matrix will depend on the transport properties of the solution,
the hygroscopicity of the matrix and is favoured by higher temperatures.
Ecient solvent extraction techniques aim to reduce mass transfer limitations to enhance rates and increase the yield. The batch
extraction kinetics during microwave assisted extraction (MAE)
shows a typical prole (Fig. 3) with dierent steps: during the equilibrium phase, solubilization and partition govern the process and
the readily accessible solute is constantly removed from the outer
Liquid
Solid
Internal diffusion
External diffusion
Solubilization-desorption
CSE
Heat transfer
Mass transfer
Heat transfer
MWE
Mass transfer
Figure 2. Mechanism of solid liquid extraction (adapted from Refs 48,
51 52).
dehydrating eect induced by rapid decompression and vaporization of water changes the surface tension of the glandular wall,
causing it to crumble or rupture more readily,51 the cell structure
is broken down and improves the capillary-porous structure of
the tissues, facilitating faster diusion out of the solid.38,61 Internal mass transport is additionally increased by microwave heating,
whereas ultrasound enhances external mass transport.49
In conventional extraction the solvent diuses through the cell
walls, dissolves and transport solutes, but tissues are slightly
damaged or remain almost intact. However, microwaves induce
changes at cellular level, which have been observed by electron
microscopy techniques. Scanning electron microscopy showed
the more rapid opening of essential oil glands of orange peel,62
their sudden rupture in thyme leaves,63 breakage and disruption in
lavender inorescences,64 and in rosemary leaves,58 and huge perforations on the surface of cardamom65 and caraway56 seeds, as
well as destructuration and attening in the inner parenchyma of
the essential oil-containing structures of orange peels.41 A similar
destruction of trichomes was observed at shorter irradiation times
than in conventional extraction of rosemary leaves.66 Evidence
of the explosive damage and destruction caused during MWE
was provided for plants,61,67 microalgae,68,69 and macroalga.70 The
reduction in particle size of microwave treated sample resulted
in an increasing specic surface area.71 Examples of SEM micrographs of the intense destruction, shrinking in some parts and
irregularities in the surface of a brown seaweed tallus and vesicles and ericaceae and gorse owers are shown in Fig. 4. Transmission electron microscopy conrmed the soybean cell wall
disintegration72 and light microscopy showed drastic structural
alterations in vacuoles compartments and destructuration in epidermal, sub-epidermal and mesophyll cell walls of onion leaves,
culminating with plasmolysis.43
TYPES OF TECHNOLOGIES USED IN

MICROWAVE ASSISTED WATER EXTRACTION
PROCESSES
The application of microwave energy may be performed operating
in: (i) pressurized equipments, under controlled temperature in a
high-pressure closed container where solvent is heated above its
boiling point; or (ii) open-systems at atmospheric pressure.15,19,42,73
The advantages of each are listed in Table 1. A number of modications have been introduced to improve microwave assisted
processes12,20,56,63,74,75 and have been compiled.13 Microwave
equipments can operate either in monomode, if radiation is
focused on a restricted zone, allowing homogeneous distribution
of energy in the cavity or in multimode, if radiation is randomly
dispersed in the cavity as a result of multiple reections on the
walls and vessel. In multimode ovens, mode stirrers are needed to
avoid nonuniform heating, which can cause the formation of hot
and cold spots.
Microwave-assisted extraction (MAE, MWE or ME) refers to
the use of microwave heat to accelerate solvent extraction processes; when water is used as the solvent, it can be added to
the solid and the slurry is treated either in open or in closed
vessels.3,16,49,60,71,72,76 83,86 This nomenclature can be referred only
to open systems15 or refer explicitly to the type of system, i.e.
open-vessel microwave extraction (OVME).84 The content in the
vessel can be stirred.85,86 Closed systems are alternatively denoted
as subcritical water or microwave superheated water extraction,86
and equipments used for synthesis have been proposed. Simplied schemes of microwave assisted water extraction (MWE) using
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surface of the particle. An intermediary transition phase can occur

before the diusion stage, which is the latter and shows lower
extraction rate, and often, the limiting step.48 The process is faster,
but the shape of the curve is similar to that of conventional extraction processes.41,51,56,57
The benets of microwave in extraction processes are in relation
to selective heating and thermal eects on the physicochemical
and transport properties of solvent and solutes, as well as the
thermal induced structural damage of the matrix.
In conventional processes, heat is transferred by convection
and conduction, whereas microwaves penetrate into the solid
at the speed of light, causing direct generation of heat within
the material and a simultaneous temperature rise.42 By adjusting
microwave output, the amount of heat energy generated inside
the solid can be controlled and heating can be relatively uniform. Since the vessels are usually made of microwave transparent
materials (borosilicate glass, quartz, Teon) the temperature gradient is inverted with respect to conventional thermal heating. The
highly localized heating caused by microwaves can induce selective migration of the solutes to the surroundings at a higher rate
than in conventional extraction. The acceleration of the microwave
extraction could be due to a synergy combination of mass and heat
transfer phenomena acting in the same direction41,58 (Fig. 2).
In addition, the change in the electric eld direction induces
rotation, vibration and swing of the molecules, intensifying the
movement and collision eciency, weakening hydrogen bonds,
which facilitates disruption of the solute-matrix interactions and
release of target compounds.59,60
During microwave assisted extraction the energy is eciently
absorbed by polar molecules and the sudden internal superheating cause liquid vaporization and pressure built up within the cells.
The severe thermal and mechanical stress and localized pressures
drastically change the physical properties of the cell walls. The
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Figure 3. Temperature and yield proles during microwave assisted water extraction processes: ( ) MAE: sulforaphane from white cabbages;53 ( ) SFME:
essential oil from thyme;54 ( ) MHG: avonoids from onion;55 ( ) MAD: essential oil from lemmon peels;51 ( ) MDG: essential oil from caraway seeds.56
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added water or solvent free are shown in Fig. 5. Most of them

are batch, but continuous operation has been reported either
pumping the slurry,69 solids,103 or by semicontinuous pumping
the liquid phase.104 106
Atmospheric solvent-free microwave-assisted extraction (SFME,
SFMAE)107 microwave assisted simultaneous distillationsolvent
extraction (MW-SDE)90 is a combination of microwave heating
and dry distillation at atmospheric pressure without any added
solvent or water. It can be achieved in a single stage in dierent
congurations, and can be performed in a modied oven adapted
to transport the steam out of the cavity.93 It has been proposed
for fresh54,65,95 and dry plant materials rehydrated by soaking in
water.57,65
Fast microwave-accelerated distillation, microwave dry distillation, MAD or DryDist combines microwave energy and distillation
and has been used for essential oils extraction without any added
solvent. The internal heating induces rupture of trichomes, frees
essential oil and the vapour condensed outside the microwave
cavity is collected. Excess water is reuxed and recycled to the
extraction vessel to restore the moisture of the plant material.51
MAD has also been applied to conventional extraction apparatus,
i.e. Soxhlet,88 Clevenger,57,62,92,98 or Vigreux column and Dean Stark
glassware.89
Microwave steam distillation (MSD), microwave assisted steam
distillation (MASD) or in situ microwave-generated hydrodistillation (ISMH), is based on the external generation of steam,
which passes through the solid bed, evaporating and carrying the
essential oil towards the condenser on the top.64,96 Microwave

steam diusion (MSDf ) is a combination of microwave irradiation
and diusion of the saturated steam, which passes through the
bed, and the mixture of extract and steam drawns naturally downwards by gravity into a condenser outside the microwave cavity.41
The extraction performed by a single stage involving the application of microwave irradiation and earth gravity is named
microwave hydrodiusion and gravity (MHG). Microwave
dry-diusion and gravity (MDG) is performed without any added
solvent or water.56 The hydrodiusion allows the extract to diuse
outside the plant material and the extract is dropped on a spiral
condenser outside the microwave cavity; water and essential oil
are collected and can be separated by density. MHG was successfully applied to the extraction of volatile compounds from fresh
plant materials with a minimum 60% of initial moisture.43,58,100 102
Vaccum microwave assisted hidrogravity (VMHG) can be performed in the same equipment by introducing vacuum; the pump
can be tted between the condenser and the ask used to collect
extract.55
Combination of microwave assisted water extraction and other
conventional or emerging physicochemical and biotechnological technologies has been proposed to favour the extraction
yields and selectivity or the thermal stability of solutes: i.e. ultrasonic/microwave assisted extraction,108,109 microwave-enhanced
vacuum ice water extraction.110 Exposure of the plant material to
microwave radiation was used as a pretreatment before vacuum
ice water extraction,110 hot water extraction,77 subcritical water
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Figure 4. Microstructural changes in the cell walls caused by microwave assisted extraction of (a) a brown seaweed tallus and (b) vesicle, (c), ericaceae
owers, and (d) gorse owers.
extraction,111 steam distillation, solvent extraction,49,93 supercritical carbon dioxide extraction68 and enzymatic incubation.112
Enzyme digestion was also perfomed before MHG extraction70 or
simultaneously with microwave-assisted aqueous.113
APPLICATIONS OF MICROWAVE ASSISTED

WATER EXTRACTION
A number of molecules have been successfully extracted either for
analytical or for processing purposes (Fig. 6), using water as the
only extracting agent.
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Analytical uses
Microwave extraction has been proposed as an alternative technique with advantages over conventional methods: reduced
extraction time and volume of organic solvents, improved eciency and selectivity, precision of analyte recoveries and good
reproducibility, with limited degradation, decreased costs and
contamination levels, avoiding additional sample clean-up and
concentration steps before chromatographic analysis.4,11,14 The

use of microwave technology as a heating source has become
common practice in laboratories, and some extraction protocols
have become standard analytical tools accepted by international
organizations.
Applications at analytical scale both in open vessel and closed
vessel devices have reported the use of water and microwave
energy in assisting extraction of environmental organic pollutants from a variety of samples, toxic compounds from foods and
bioactives from plants. The microwave-assisted extraction of polycyclic aromatic hydrocarbons from solid matrices (soils and sediments) and plant materials is an ecient and low cost method.
Water is a good alternative to organic solvents for MAE of nicotine from mushroom,106 pesticides and herbicides from soil114 and
insecticides from vegetable and soil samples.115 Given the variable bioavailability and toxicity of dierent As species, an appropriate analytical tool is needed to characterize foods. Aggressive
reagents commonly used for total arsenic extraction,116 do not
give the precise characterization of species, but water can provide
a similar eciency preserving As speciation from rice,117 brown
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Table 1. Comparative advantages of the open and closed congurations

Open
Closed
Operation at atmospheric temperature

Safety
Milder conditions, suited for thermolabile compounds
Higher sample throughput
Possibility of adding solvent to the system during the process
Reduced solvent consumption
Precise control of the energy delivered to the sample
Easy removal of excess solvent from the extract
No requirement for cooling down or depressurization
Lower investment in the equipment
Low cost and easy automation of the equipment required
No further clean-up steps required before analysis
Vessels made of various materials can be used
algae,118 sh and shellsh,119 and plankton.120 Another example is

the extraction of mycotoxins at temperatures up to 150 C without
degradation.78
The characterization of secondary metabolites from medicinal
plants has helped in the discovery of new drugs. The renewed
interest in natural remedies emerged since modern medicine is
not capable of providing a cure to all diseases and herb extracts
contain multiple active constituents, which can act synergistically,
providing unique therapeutic properties with minimal undesirable
side-eects.14 However, the lack of consistency, safety, and reliable analytical techniques, limits the standardization and quality
control of herbal materials. Microwave extraction has grown as a
promising technique for extraction, clean-up, and concentration
of phytochemicals,14,75 for providing distinctive chemical ngerprints for quality control60,121 or for routine analysis.59,62,90
Extraction of compounds from plants
Microwave assisted extraction can be an optimum choice for the
extraction of plant components (Table 2). Most works deal with
the extraction of oils, polysaccharides, proteins and phenolics.
The MWE yields, eciency and selectivity are also higher than
with conventional technologies for the extraction of organic acid,
alkaloids, isothiocyanates.53,121,129,132
In the extraction of plant bioactive compounds, conventional extraction methods with organic solvents, water and
their mixtures require long extraction times, relatively high solvent consumption and could cause thermal degradation of the
phyto-constituents. Recent developments include pressurized
solvents, ultrasound-assisted extraction, and microwave-assisted
extraction, which is the simplest and the most economical. In
addition, the domestic microwave can be used to prepare aqueous extracts of medicinal plants in few minutes with eciencies
comparable with those of conventional systems. It is estimated
that more than 80% of the worlds population cannot aord
modern medicines, but due to their pharmacological safety, plant
bioactives could be used alone or as adjuncts to current agents to
enhance therapeutic eects and minimise toxicity.2
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Lipids
Although organic solvents are conventionally used to extract lipids
from seeds, alternative aqueous processes have been developed
in recent decades, particularly those using hydrolytic enzymes to
Shorter operation times than in open vessel systems

More precise methods than those in open-vessel systems
Simultaneous processing of many samples
Possibility of using higher temperatures than open system
Loss of volatile substances is virtually completely avoided
Since no evaporation occurs, less solvent is required than in open systems
Lttle or no risk of airborne contamination
The fumes produced are contained within the vessel, and provision for
handling potentially hazardous fumes is not needed
break the cell walls.133 Microwaves can aid in this process, and
pumpkin oil extracted in microwave systems showed a higher content of linoleic acid than Soxhlet extracted oil and stronger antioxidant activities.113 Microwave heating was also used a preliminary
step to disrupt the lipid body structure and release the oil from
corn germ by colloid milling and aqueous enzymatic digestion.134
Microwaves can assist in olive oil extraction to reduce time and
improve the energetic eciency, preserving the quality of the
oil.135
Some species of microalgae have high oil content (more than
80% d.w.). Oil extraction from these high water containing materials at a cost ecient industrial scale is desirable. Microwaves
are a suitable pretreatment for microalgal cell disruption facilitating the extraction with conventional solvents.68,136 A continuous
MWE method was developed for oil extraction from a green algae,
which was mixed with water and the paste was pumped through
the microwave focusing cavity. The microwave system oered a
10-fold increase in heating rates and extraction yields compared
with a control, and the oil contained higher percentages of 3 and
6 unsaturated fatty acids than that extracted by Soxhlet.69
Polysaccharides
Polysaccharides, widely distributed in animals, plants and microorganisms, possess varied biological activities. Conventional
aqueous extraction by heating, boiling, or reuxing, is a simple and safe method, but requires long extraction time and high
temperatures, that could cause degradation of polysaccharides
and decrease their pharmacological activity. Microwave irradiation using only hot water allows milder reaction conditions, which
oer lower production costs, minimization of wastes when compared with the use of alkalis, and maintains the physicochemical
characteristics of crude polysaccharides. It has been reported for
a variety of matrices including corn pericarp,137 wheat bran,138,139
ax shives,123 tamarind kernel,140 mulberry leaves,61 brewers
spent grain,86 watermelon rinds,83 tea ower,125 mushrooms,77 or
traditional Chinese medicinal plants.67,82,122 The control of MWE
extraction conditions is important to limit hydrolytic cleavage of
polysaccharide chains or alter the compositions that would enrich
in some monomers.80 Solubilization of hemicelluloses during
fractionation of lignocellulosic materials can be addressed in the
rst stage of bioreneries141 and aqueous based processes are
a promising conversion option for feedstock with high moisture
content since no drying step is necessary. Microwaves are eective
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Figure 5. Examples of congurations for microwave assisted water extraction: (a) closed vessel,3,39,60,78,80,85,87 (b) open focused systems with added water
and multimode with or withour added water, 46,49,51,54,57,61,62,65,67,71,76,79,83,84,89 99 (c) steam distillation,64 (d) MHG 43,55,56,58,96,100 102 and MDG,56 (e)
MSDf,103,41 (f ) JFE. 1. Microwave oven, 2. Cooler, 3. Steam generator, 4. Receiving ask, and 5. Vaccum pump
for the extraction and depolymerization of polysaccharides from

microalgae, facilitating disruption of the cell walls and the release
of the lipid fraction without hydrolysis of the triglycerides.142
MW technology was used for the isolation of non-degraded agar
with fairly uniform structure and enhanced gelling properties in
comparison to commercial ones81 and for the solubilization of
fucoidans from supercritical carbon dioxide deoiled wakame.87
Protein
Both the extraction and hydrolysis of protein can be enhanced
by microwave irradiation. Microwave irradiation, either to previous or simultaneously with enzymes, accelerates the enzymatic
digestion of proteins, enhancing the disruption of cell membranes and reducing the extraction time from several hours to
some minutes,72 and can also facilitate the release of protein
bound-minerals.131
597
Phenolics
Phenolic compounds are being extensively studied for the
organoleptic characteristics they confer to vegetable food
products, for their bioactive properties and were proposed as
biomarkers in quality control of medicinal herbs.121 Cell wall
phenolics are thought to have important roles in providing

mechanical strength, regulation of growth and morphogenesis,
and responses to stresses and pathogens. Phenolics are widely
found in plants and in residues of food processing. Alcohols and
acetone are frequently used, but for food purposes biorenewable
solvents are preferred, particularly water and ethanol. However,
ethanol extraction requires long processing times and oers low
selectivity. Microwave extraction using water as solvent was as
ecient as conventional processes to extract phenolics from
medicinal plants,49,79,143,144 pine seeds,3 beans,145 buckwheat,85
green coee,146 and olive leaves97 and oered yields comparable with decoction and higher than infusion and USAE for the
extraction of sennosides.84 Microwave assisted extraction in
household ovens improved the extraction of phenolics,38 catechins and caeine, without aecting the extraction of theanine.127
Water was used as solvent during MAE of phenolics from such
residues as pomegranate peel126 and fruit hulls of tea-oil tree,99
and solvent-free MHG extraction provided extracts from sea buckthorn juice by-products with higher phenolic content,147 and more
active antioxidants from onion byproducts55 than conventional
solvent extracts. Pressurized extraction at 230 C was successfully
proposed to process tea residues and to extract pyrogallol and
guaiacyl units, from the degradation of catechins and lignin,
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Figure 6. Examples of some natural compounds successfully extracted with water based and with solvent free microwave assisted extraction processes.
respectively.148 Depite the degradation occurring at these conditions, the total phenol content increased by depolymerization of
higher molecular weight phenolics. However, since a linear correlation between molecular size and activity cannot be established,
adequate optimization for each material and biological activities
should be performed.
598
Essential oils
Essential oils are aromatic mixtures of more than 200 compounds,
widely used in cosmetic, pharmaceutical and food applications.
They contain a volatile fraction (9095%) composed of monoterpenes and sesquiterpene hydrocarbons, their oxygenated derivatives, aliphatic aldehydes, alcohols and esters, and a non-volatile
residue (510%) composed of hydrocarbons, fatty acids, sterols,

carotenoids, waxes, coumarins, psoralens and avonoids. Terpenes are mostly unsaturated compounds, readily decomposed
by heat, light and oxygen to compounds conferring o-avours
and o-aromas. The traditional methods to extract essential oils,
including distillation (steam distillation or hydrodistillation), cold
pressing and solvent extraction have some disadvantages. Cold
pressing causes a gradual diminution in terpene alcohols contents and conditions favourable for hydrolysis, oxidation and
resinication are created during agitation. The elevated temperatures and prolonged times during distillation can cause modications and losses of the most volatile molecules and demands
high energy and solvent consumption.56 Steam distillation (SD)
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Table 2. Some examples of compounds extracted by microwave assisted water extraction processes
Source (compound)
Polysaccharides
Brewery spent grains
Chinese plant
Flax shives
Grapefruit peels
Macroalgae
Mulberry leaves
Spent coee grounds
Stevia
Tea ower
Watermelon rind
Phenolics
Buckwheat
Camelia
Chinese plants
Mandarine peels
Onion
Pine seeds
Pomegranate peels
Rosemary
Senna leaf
Shiso leaves
Tea
Terpenoids
Black cummin seeds
Caraway seeds
Cardamon seeds
Citrus peels
Lavender owers
Spices
Oreganum
Alkaloids
Cacao
Chinese plant
False calumba
Minerals
Yeasts (Se)
Medicinal plants (Se)
Technique: LSV Ratio

(g/mL/mL)b
Ref.
2
20.8
10
6
5
20
5
20
52
2.1
MWE: 10/60/100
MAE: 1/22/50
MAE: 1/27/MAE: 6/300/MAE: 1/20/MAE: 10/150/MAE: 8/80/100
MAE: 0.2/20/50
MAE: 50 /400/1000
MAE: 1/20.3/250
86
122
123
124
81
61
80
60
125
83
150
76
80
135
100
125
-
15
35
40
3
20
20
1
7d
5
23
1e
MAE : 1 / 50 / 100
MAE: 10/153.3/500
MAE: 10 / 100 / MAE: 1/14/100
MHG: 500/-/1000
MAE: 1/25/MAE: 1/20/MAE: 25/150/MAE: 3 / 10 / MAE: 1/ 16.5 /MAE: 2 / 200 / 250
85
99
71
39
101
3
126
49
84
79
127
350
100
390
500
200
622
100
100
100
-
10
45
75
15
6
60
20
MAE: 25/25/250
MDG: 200 / - / SF: 100 / pmf /
MHG 500 / - / MSD: 20/ ng/ SF: 250 /pmf / SF: 50/145/1000
92
56
65
100
64
128
57
210
600
-
120
160
5
20
15
MAE: 0.5/90/MAE: 0.5/20/MAE: 1/40/-
129
121
130
60
900
37
15
2
MAED: 0.04 / 2 / 2.5

MAE: 1 / 25 / 50
131
2
P (W)
T ( C)
900
60
700
750
477
140c
101
180
90
60
200
100
-
500
700
400
500
600
250
500
600
500
t (min)a
MWE: Microwave superheated water extraction; MDG: Microwave dry diusion and gravity; MHG: Microwave hydrogravity; SF: Solvent free microwave
extraction; MSD: Microwave steam distillation; MAED: microwave assisted enzymatic digestion.
a number of stages.
b solid/liquid/vessel ratio, in solvent free techniques, the name is indicated.
c further reextracted.
d on-o periods of 0.5 min.
e performed after 0.54 min boling.
f previously moistened.
g not added.
and advantages such as selectivity, shorter extraction time and

energy saving,76 which limits the degradation of thermolabile
compounds.54,57,65,149 Solvent free produced extracts of origanum
contained more thymol (81.1%), compared with typical microwave
process (65.4%) and conventional hydro-distillation (41.6%).
Microwave assisted extraction processes can be completed in
1230 min compared with 13 h for conventional technologies
(Fig. 7). Also, microwaves as a pretreatment before conventional
599
is widely used and the losses of thermolabile compounds could

be limited operating at reduced pressure.104 Hydrodistillation (HD)
remains the most common method both in the laboratory and on
an industrial scale.
Dierent alternatives have been proposed for the application
of microwave dielectric heating for the extraction of essential oils from aromatic herbs and spices,51,91 with quality and
yield similar to those obtained using conventional techniques,
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Figure 7. Comparison of extraction time, energy consumption and CO2 emitted in hidrodistillation ( ) and microwave hydrogravity ( ) processes.
HD reduced extraction time, saved energy, and prevented volatile

loss.66
There is no signicant dierence between the physical properties and the aromatic prole and compositions of the essential oils isolated by microwaves and by conventional techniques,
from aromatic herbs and spices extracted by SFME and by conventional HD,128 from orange peels by MSDf and SDf,41 from berries
using microwave turbo hydrodistillation74 and from mint leaf by
HD and in situ MGH,41,102 but the MAD method oers better reproduction of the natural aroma than that obtained using CP or
HD.51,56 58,62,63,89,100
Other authors reported that the essential oils extracted by
MAD and by SFME are more valuable because they contained
a higher fraction of oxygenated compounds, responsible for the
odoriferous properties of essential oils, and lower fractions of
monoterpene hydrocarbon than those obtained with HD and
CP.13,62,65,91,95,102,128 (Fig. 8) The rapid MW heating of the polar substances and the lower water content can prevent thermal and
chemical decomposition of compounds by hydrolysis, transesterication or oxidation,13,62,98 although some oxidation reactions are
promoted by the MW irradiation, resulting in a rise of oxygenated
compounds and darker color of the SFME essential oils.98
A general trend in the variation of the amounts of monoterpene hydrocarbons and sesquiterpenes with extraction time was
observed. Monoterpene hydrocarbons, relatively volatile and
unstable against heat and light, were preferentially extracted in
the earlier periods whereas sesquiterpenes, with higher molecular weight compounds less volatile and soluble in water were
extracted in the nal stages.57 The oil composition is inuenced
by two mechanisms, hydrodiusion and MW polarization could
act simultaneously or in combination:91,102 (a) microwaves interact
with the free water molecules in the plant glands and vascular
systems and the expansion undergone upon heating causes
subsequent rupture of the tissue. The essential oil dissolves in
water and the dierences in oil composition are related to the
water solubility of the components; (b) organic compounds with
600
Figure 8. Comparative composition of essential oils obtained by conventional and microwave solvent free processes.

higher dipolar moment can be extracted more readily due to their
stronger interaction with the MW irradiation than compounds
with low dipolar moments.65
VARIABLES AFFECTING THE MICROWAVE

ASSISTED WATER EXTRACTION
The MW extraction of vegetal compounds is inuenced by the
properties of the matrix, the solute, the solvent and the operational conditions.16 18,73 The eect of the most inuential
variables when water is used as solvent is summarized in this
section. Due to the multivariate character of MWE processes,
experimental design and response surface methodology proved
useful.39,41,61,65,72,79,82,83,99,109,122,129,137,151
Temperature
Elevated temperature values usually enhance yields as a result
of increased diusivity of the solvent into the matrix and desorption and partition of solutes into the solvent. However, temperature should be controlled to avoid formation of by-products,
decomposition and/or degradation. In closed systems, temperature can increase above the normal boiling point and significantly alter the properties of water.8,121 During MWE increasing yields up to an optimal value were observed, i.e. up to
6070 C for water-soluble polysaccharides from bulbs of Chinese plants.82,151 Operation at higher temperatures (170200 C)
during shorter times could facilitate industrial implementation
and the yields of arabinoxylans and arabinoxylo-oligosaccharides
increased in the range 140210 C from spent coee grounds,80 at
190210 C from brewers spent grains86 and at 150185 C from
wheat bran.139 However, the recovery was reduced due to depolymerization, debranching and deesterication and the composition and structural variability was dependent on the extraction
conditions.86,139
The phenolic content and antioxidant activity of buckwheat
extracts increased from 23 to 150 C.85 Although at 180 C extraction is facilitated, compounds are susceptible to undergo Maillard reaction products, with enhanced antioxidants properties,39
but both the colour and physical appearance can be aected and
bioactivity decreased.3 The optimum temperature diers for dierent phenolic molecules, i.e. in the range 40120 C the extraction
of epicatechin from uncaria increased whereas the recoveries of
catechin and caeic acid decreased.121 The degradation of phenolics at 50175 C can be induced by light and air79,146 and by
the type and number of substituents.152 154 Information on the
degradation of other components during microwave heating is
available, i.e. vitamin B12 ,155 anthocyannins156 or undesirable compounds, such as Ochratoxin A78 and arsenic.117 Temperature is
closely related to the irradiation power and their inuence should
also be considered in relation to the extraction time.
Typically, increases in extraction yield with irradiation power

have been reported, i.e. up to 350600 W for periods up to 70 min
for water soluble polysaccharides from bulbs,82,151 and up to 480 W
for pectin extraction from watermelon rinds.83 However, irregular
variation on the yield of tea ower neutral and acid saccharides
with irradiation power from 550 to 750 W has been observed.125
The eect of irradiation power was more signicant at shorter
times.79 Increasing power enhanced the yield of phenolics from
dierent sources but degradation may occur at higher wattage.
Optimal values were 400800 W at 5 min for chlorogenic acid
and caeine from green coee plants,146 600 W in 23 min for perilla leaves avonoids,79 500 W at 26 min for onion phenolics,101
900 W and 3 min for tea phenolics,38 1000 W and 45 s for cherries anthocyanins,107 500 W for maize avonoids,153 and 90210 W
were chosen to avoid losses of theobromine and caeine from
cacao129 and 160500 W for cassia sennosides.84 The specic
power density could oer more suitable information, values of
12 W g1 have been frequently found as optimal.51,55,70 Lower
power inputs can also be useful, i.e. to attain the maximum yields
for essential oils at 85600 W91 or selenium from yeasts increased
with power up to 60 W in 30 min.131
Extraction time and cycles
Time is a key factor in microwave assisted extraction processes,
with an initial positive impact on the yields, and beyond an optimum value, the yield stabilizes or slightly decreases if degradation
of solutes and/or excessive breakage of the oligomeric fractions
occur. In operation with short periods, heating time should be
considered, i.e. come-up time to treatment time ratios of 1/3 for
buckwheat,85 1/8 for corn starch industrial waste,137 3/2 for coee
grounds80 were reported. Optimal values can be usually attained
in 0.55 min for pectin from watermelon rinds,83 polysaccharides
from spent ground coee80 and from brewers spent grain,86 sennosides from cassia,84 chlorogenic acid and caeine from green
coee,146 phenolics from mandarin39 and pomegranate126 peels,
and from Melissa,143 anthocyanins from cherries,107 catechins from
tea,127 essential oil from clove basil,157 water extractable Se from
medicinal plants,2 and sulforafane from cabbages.53
Decreased yields due to degradation were observed for more
than 1020 min with hemicelluloses from ax shives,123 organic
acid and alkaloids of uncaria,121 phenolics from melissa143 and
avonoids from onion,101 showing a dierent prole of the constituents with dierent glycosidic substituents. However, longer
times have also been recommended, i.e. 76.8 min for polysaccharides from silverweed at 369 W and 63.3 C151 and 60 min at 50 C
and 597 W for those from lilium,82 35 min for polyphenols from
oilseed camelia at 76 C,99 and 30 min for green tea avanols,158
soluble proteins in soybeans.72 Periods between 10 and 70 min
were optimal for essential oil extraction.13,91 The lipid yield from
a green alga increased steadily at 8095 C for 30 min, the percentage of oleic acid increased during 20 min and then decreased,
whereas unsaturated fatty acids increased.69
The extraction time can be reduced by operating at increased
power (Fig. 9). The favourable inuence of power from 50 to 150 W
during the extraction of terpenes from caraway seeds was more
marked at short times.159 Controlling microwave power at short
irradiation time (300700 W and 30120 s) at mild temperatures
of 100120 C gave better results than temperature-controlled
extraction of antioxidant polyphenolics from henna leaves.160
The use of on/o cycles was reported49 during operation at a
constant temperature 140 C with dierent power inputs, and a
slight eect of power was observed in the recovery of onion
601
Power
Increasing microwave irradiation energy can enhance the molecular interaction of the electromagnetic eld and the materials, facilitating the penetration of solvent into the plant matrix and the
dissolution and recovery of solutes. Power setting must be chosen
correctly to maximize yields, selectivity and stability of the target
solutes, especially in closed vessel systems, to avoid overpressure
and excessive temperatures. Pressure is a key variable for closed
vessel extraction, but it is directly dependent on the temperature,
which is usually the preferred controlled variable.60
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Figure 9. Relationship between irradiation power and time in microwave

assisted water extraction processes.
avonoids at 300900 W,101 and phenolics from mandarin peels at

400800 W.39
The application of a sequence of cycles has been proposed for
the extraction of selenium from yeasts,131 phenolics from shiso
leaves,79 cherries107 and brown seaweed.70 The application of consecutive stages at increasing severity was proposed for the extraction of galactomannans and arabinogalactans from spent coffee grounds80 and arabinoxylans or arabinoxylo-oligosaccharides
from wheat bran138 and from brewers spent grains.86
Nature of the matrix and moisture content
The water content in a plant sample has great inuence on the
extraction eciency, since the high dipole moment of water
molecules is decisive in the sample heating, and subsequent
physicochemical phenomena favouring solvent extraction with
water and also with other non green solvents.161 163 The eect
of moisture is dependent on the nature of the sample and the
presence of water enhanced the extraction of some compounds,
but reduced the recoveries of others.164 The water content of
the matrix should be controlled to obtain reproducible results
although some pretreatment of the material can lead to broken
structures that can no longer hold water. The non-homogeneous
dielectric heating throughout the material, could also induce the
formation of hot and cold spots. Signicant increase in extraction
eciency was observed when a small amount of water was added
to the plant materials prior to microwave extraction, and 67% was
found to be optimal for SFME of cardamom;65 herbs can be soaked
before solvent free microwave extraction, and they can absorb
near 300% of their initial weight.57,65,128
602
Solvent to solid ratio

In conventional solvent extraction limitations derived from solubility or mass transfer occur at lower solvent:solid ratios, the
extraction yield increases with the increase in the solvent:solid
ratio, but above an optimal value no additional improvements are
observed and would provide too diluted extracts. In MW assisted
aqueous processes, the solvent to solid ratio could have additional
implications for the yields and stability of the target products due
to the ability of water to absorb energy and the need for uniform
distribution and exposure to microwaves.18,48 In MAE processes
the lower yields observed with lower solvent:sample ratio could
also be related to the decreased surface area available for the

solvent, the plant materials absorb and disperse more energy
near the surface and the incident radiation per particle decreases,
reducing the eect of microwave irradiation by lower penetration into the suspension. The reduction in extraction yield with
increasing liquid/solid ratio can be observed depending on how
the solvent:solid ratio is changed. Maintaining the solvent volume
constant, the temperature of the suspension remain almost constant and the extraction yield is enhanced at higher solvent:solid
ratios, but if the solid mass is constant and the solvent volume is
increased, the temperature of the mixture is determined by the
dielectric properties of the sample and for higher solvent:solid
ratios longer heating times are required to reach the same temperature, and lower recoveries were obtained.38,165 Besides the
physical properties of the contents of the reaction vessel, both the
volume of the contents and geometry of the reaction vessel are
crucial to provide uniform and reproducible heating.8
The inuence of dierent ratios of water to raw material on
the polysaccharides yield usually showed an optimal value, i.e.
10 for spent coee grounds,80 16.9 for orange peels,166 20.3 for
watermelon rinds,83 25 for fungi polysaccharides77 and 65 for lily
bulbs.82 The lower liquid to solid ratios did not result in higher
recovery of the polysaccharide but only of the monosaccharides,
and the concentrated conditions promoted a higher extension
of degradation of the spent coee polysaccharides.80 Optimal
solid/liquid ratios for phenolics were reported: 10 from a Chinese
plant,71 14.5 from potentilla,151 15.3 from camellia,99 20 from
pomegranate peel,126 25 from pine seeds3 and vanilla bean,167 30
from melissa143 and more than 40 from tea.38 Relatively low values
were found to be optimal for the extraction of other components,
10 for dimethylarsenic from rice117 and 12.6 for soluble soybean
protein.72 However, when the amounts of solid and liquid were
simultaneously varied with the same heat load per unit mass, the
solid to solvent ratio does not have a large eect for water to citrus
peel ratios from 2 to 45.39
Other variables
The variation of pH during water based microwave assisted extraction has been observed in relation to the release of acidic substituents by the hydrolysis of esters of ferulic and acetic acids or by
the thermal degradation of sugar residues that can be converted
into formic and levulinic acids during the autohydrolysis process.
The pH values decreased gradually with the increase of severity,
and may contribute for the higher yields at higher temperatures.
The optimal initial pH for pectin, 1.4166 or 1.5283 was selected to
maximize yields and to avoid aggregation of pectin. Selection as a
function of the stability of solutes, avoiding oxidation of phenolics
was also proposed.79 The inuence of the type of digestion system
was reported in relation to the particle size, when this variable was
limiting. The extraction eciency of arsenic from rice was higher in
closed than in open vessels when the particle size was larger than
0.5 mm, but no dierence was observed for powdered samples.117
SCALE-UP, ENVIRONMENTAL IMPACT,

ENERGETIC AND COST ASPECTS
In a recent survey on manufacturing processes for pharmaceutical ingredients and intermediates, microwave heating was still
regarded as a novelty mainly due to the perceived diculty of
scaling up microwave reactions.25 Regarding microwave assisted
extraction, most literature reports on microwave extraction
are for small-scale systems, but approaches to scale up proved

feasible6,20,91 and some MWE processes could be performed
in existing extractors.62,101 Industrial application has potential
benets,25,146 based on improvements in product eciency, process enhancement and low maintenance costs achievable on a
commercial scale.
The energy eciency of microwave heating is case dependent.
Abundant information on the cost of extraction of essential oils for
microwave assisted techniques compared with conventional HD
and SD is available. The reduced cost of extraction of microwave
processes for essential oil is clearly advantageous over conventional processes in terms of energy and time required to attain
similar yields, quality and properties.94,166 The energy required to
perform MAD (electrical energy for microwave supply) is lower
in relation to that required for HD (electrical energy for heating and evaporation), and CP (electrical energy for a mechanical motor).51,56,89,102 The energy required to perform conventional
extraction processes is 1.617 times higher per gram of essential
oil than for a microwave assisted process (Fig. 7(b)).
Preliminary studies indicate that the cost of microwave based
processes could be competitive with traditional SD of essential oils
although two major disadvantages have been described: (i) high
investment cost of the continuous microwave oven; and (ii) higher
cost of electricity than fuels. In a perspective paper a critical assessment revealed that heating in the microwave-assisted transformations performed in laboratory single-mode microwave reactors
is energy inecient, and its green, sustainable and environmentally friendly character is questionable. However, when scaling up
and moving from single-mode to multimode reactors, microwave
heated processes can be more energy ecient than conventionally heated equipments5 . Similar eects would be expected in
extraction and the use of specialized microwaves allows easier
and proper control of operation, and lower cost than pressurized
extraction.48
One of the most relevant aspects in relation to environmental
impacts is the carbon footprint or the total amount of greenhouse
gas emissions, assessed in carbon dioxide units, caused directly
and indirectly by the process and calculated considering that to
obtain 1 kWh during combustion of fossil fuels, 800 g of CO2 will
be emitted to the atmosphere. The calculated carbon footprint
for solvent free MW assisted extraction of essential oils is shown
in Fig. 7(c), with values of 520% of those obtained with conventional distillation.20,41,51,89,102 MAD is a clean method, which avoids
the residue generation (as in CP) and the use of a large quantity of
water and voluminous extraction vessels (as in HD).51,62 Furthermore, the waste waters rejected were 85 L kg1 essential oil for
MSDf against 290 L kg1 essential oil for SDf.41
CONCLUSIONS
systems could make MWE a popular extraction method for a wide

variety matrices and natural products, with special attention given
to environmental applications and to obtain consistent, safe, and
ecient herbal products.
ACKNOWLEDGEMENTS
The authors are grateful to the Ministry of Science and Innovation of Spain (Research Projects Ref. CTM2009-12664 and
CTM2012-38095) for nancial support of this work.
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Microwave assisted water extraction (MWE) of valuable components from renewable raw materials conforms with the principles
of green extraction, to obtain high quality extracts from plants.
Microwave processing is advantageous over conventional techniques, due to the faster and selective heating, shorter extraction
time, in safe, robust, simple and controlled processes with higher
extraction eciency and minimum degradation of target components avoiding residue generation and the use of large quantities
of water. MWE is an ecient environmentally friendly technique
for both analytical and processing purposes, the possibility for
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Microwave Assisted Water Extraction of Plant Compounds

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Microwave Assisted Water Extraction of Plant Compounds

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Review

Received: 20 June 2014

Revised: 12 August 2014

Accepted article published: 19 August 2014

Published online in Wiley Online Library: 22 September 2014

(wileyonlinelibrary.com) DOI 10.1002/jctb.4519

Microwave assisted water extraction

Recent trends in chemical design of manufacturing processes have

microwaves was critically reviewed.21 In the last decade a number

WATER AS A GREEN EXTRACTION SOLVENT

2014 Society of Chemical Industry

Microwave assisted water extraction of plant compounds

J Chem Technol Biotechnol 2015; 90: 590607

water was initially used to extract contaminants from soils and

FUNDAMENTALS OF MICROWAVE HEATING

2014 Society of Chemical Industry

Finding and recognizing a green solvent, an easily-removable

(infrared radiation), which correspond with wavelengths from 1 m

N Flrez, E Conde, H Domnguez

MECHANISM OF MICROWAVE ASSISTED

2014 Society of Chemical Industry

J Chem Technol Biotechnol 2015; 90: 590607

Microwave assisted water extraction of plant compounds

J Chem Technol Biotechnol 2015; 90: 590607

TYPES OF TECHNOLOGIES USED IN

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surface of the particle. An intermediary transition phase can occur

N Flrez, E Conde, H Domnguez

added water or solvent free are shown in Fig. 5. Most of them

essential oil towards the condenser on the top.64,96 Microwave

2014 Society of Chemical Industry

J Chem Technol Biotechnol 2015; 90: 590607

Microwave assisted water extraction of plant compounds

APPLICATIONS OF MICROWAVE ASSISTED

J Chem Technol Biotechnol 2015; 90: 590607

2014 Society of Chemical Industry

concentration steps before chromatographic analysis.4,11,14 The

N Flrez, E Conde, H Domnguez

Table 1. Comparative advantages of the open and closed congurations

Operation at atmospheric temperature

algae,118 sh and shellsh,119 and plankton.120 Another example is

Shorter operation times than in open vessel systems

2014 Society of Chemical Industry

J Chem Technol Biotechnol 2015; 90: 590607

Microwave assisted water extraction of plant compounds

for the extraction and depolymerization of polysaccharides from

J Chem Technol Biotechnol 2015; 90: 590607

2014 Society of Chemical Industry

phenolics are thought to have important roles in providing

N Flrez, E Conde, H Domnguez

residue (510%) composed of hydrocarbons, fatty acids, sterols,

2014 Society of Chemical Industry

J Chem Technol Biotechnol 2015; 90: 590607

Microwave assisted water extraction of plant compounds

Technique: LSV Ratio

MAE: 0.5/90/MAE: 0.5/20/MAE: 1/40/-

MAED: 0.04 / 2 / 2.5

J Chem Technol Biotechnol 2015; 90: 590607

and advantages such as selectivity, shorter extraction time and

2014 Society of Chemical Industry

is widely used and the losses of thermolabile compounds could

N Flrez, E Conde, H Domnguez

HD reduced extraction time, saved energy, and prevented volatile

2014 Society of Chemical Industry