Food Quality and Safety, 2017, 1, 61–81

doi:10.1093/fqs/fyx004
Review

Review

Recent advances in extraction of antioxidants

from plant by-products processing industries
M. Selvamuthukumaran* and John Shi**

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*Department of Food Science and Post Harvest Technology, Institute of Technology, Haramaya University, PO Box
138, Dire Dawa, Ethiopia and **Guelph Research and Development Center, Agriculture and Agri-Food Canada,
93 Stone Road West, Guelph, Ontario N1G 5C9, Canada

Correspondence to: M. Selvamuthukumaran, Department of Food Science and Post Harvest Technology, Institute of Tech-
nology, Haramaya University, PO Box 138, Dire Dawa, Ethiopia. E-mail: msm_foodscience@yahoo.co.in
Received 21 October 2016; Revised 28 December 2016; Editorial decision 30 December 2016.

Abstract
The by-products obtained from plant processing industries are the cheap source of bioactive
compounds especially antioxidants. Extraction of bioactive compounds can be obtained by using
conventional and non-conventional methods. Extraction efficiency of any conventional method
mainly depends on the choice of solvents. The major challenges of conventional extraction are
longer extraction time, requirement of costly and high purity solvent, evaporation of the huge
amount of solvent, low extraction selectivity, and thermal decomposition of thermolabile
compounds.To overcome these limitations of conventional extraction methods, new and promising
extraction techniques are introduced. These techniques are referred as non-conventional extraction
techniques. Therefore, in this review, some of the most promising techniques such as ultrasound-
assisted extraction, pulsed electric field extraction, enzyme-assisted extraction, microwave-assisted
extraction, pressurized liquid extraction, supercritical fluid extraction, pressurized low-polarity
water extraction, and molecular distillation were discussed. The process systems along with
industrial applications for non-conventional method of antioxidants extraction were discussed,
and the comparative efficacies of different extraction methods were highlighted. Replacing
conventional technologies by non-conventional ones for the extraction of valuable compounds
from plant by-products processing industries has several advantages, which includes reduction
of the processing time, energy consumption, and the uses of harmful and expensive solvents and
increase in the extraction yields. Incorporation and development of hybrid methods should be
investigated, while considering plant material characteristics and choice of compounds in future.
Proper choice of standard methods also influences the measurement of extraction efficiency. The
increasing economic significance of bioactive compounds and commodities rich in these bioactive
compounds may lead to find out more sophisticated extraction methods in future.

Key words: Antioxidants; Extraction; Non-conventional methods; Plant by-products; Pulsed electric field extraction; Ultrasound-
assisted extraction.

Introduction 1989; Ajila et al., 2010). The tissue portion obtained from underuti-
lized plant materials was the rich source of several antioxidant com-
The non-edible portion obtained from plant by-products ranges
ponents viz. polyphenols, carotenoids, flavonoids, anthocyanins, and
from 25 to 30%, and the inability to recycle such products will
vitamins (Ayala-Zavala et al., 2004). Fruits and vegetable processing
significantly contribute to a huge economical loss (Bhalerao et  al.,

© The Author 2017. Published by Oxford University Press on behalf of Zhejiang University Press.
61
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62 M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1

unit delivers several unutilizable waste materials, which comprises
mainly seeds, peel, and stones. Among them, the fruit peel exhib-
ited significant antioxidant activity, which is around 2- to 27-fold
higher than fruit pulp (Someya et al., 2002; Guo et al., 2003; Goulas
and Manganaris, 2012). The inexpensive source of antioxidants was
reported to be obtained from by-products of several fruits viz. star
fruit (Shui and Leong, 2006), grapes (Lafka et al., 2007), citrus fruits
(Xu et al., 2008), and pomegranate (Singh et al., 2002).
The crude extracts obtained from several plant materials were the
rich source of phenolic compounds, and they have potential applica-
tion as preservatives and also used in development of several func-
tional foods and nutraceuticals (Marja et al., 1999). Therefore, the
consumption of antioxidant rich foods will scavenge the formation
of free radicals, and it also helps in preventing the oxidative stress-
functional food products. Higher antioxidant extraction methods
are available for use at a commercial level. These methods were
found to be safe, eco-friendly, and possess non-carcinogenic effect
when compared to synthetic methods. The production/recovery of
high-value compounds such as antioxidants is increasingly being
considered through the biorefinery concept Bozell and Petersen
(2010). Therefore, in this review, the recent methods in extraction
of antioxidants from plant by-products processing industries were
discussed, and commercial method of antioxidants extraction at a
large-scale level and also comparative efficacy of different extraction
methods were highlighted. The process systems along with industrial
applications for non-conventional method of antioxidants were dis-
cussed. Therefore, the food industry can choose the efficient method
of extracting functional components from several plant by-products

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related diseases (Joshi et al., 2012). Fruits and vegetables found to
possess several non-digestible components and phytoconstituents
in the form of antioxidants, which significantly contribute towards
the several added health benefits. These antioxidants are nowadays
widely used as functional ingredients in many processed foods. The
marketing trend in this field is quiet competitive, and therefore, the
development of new type of quality ingredients is a big challenge for
the food processing industries.
The term ‘by-product’ means reusuable plant wastes, which are
having a good market value (Sanchez-Zapata et al., 2009). Globally,
the large amounts of plant wastes were generated from several food
processing industries, which were estimated to be around 800 000
t/year (Ayala-Zavala et  al., 2010). The wastes obtained from such
industries are highly perishable, and they will pose serious environ-
mental problems to society (Arvanitoyannis and Varzakas, 2008).
Table 1 shows the by-products generated from fruits and vegetables
processing industries, and these by-products comprises mainly of
skins, seeds, stems, leaves, wastewaters, and unusable pulp, which
are normally discarded after processing (Ajila et al., 2007). These by-
products amount contributes to more than 40% for plant foods such
as artichoke, asparagus, cactus pear fruit, mango, orange, papaya,
pineapple, red chicory, and tiger nuts.
The plant by-products are considered to be one of the cheap
sources of several antioxidants. The extraction of antioxidants
from such plant by-products is very much essential for developing
on a large-scale basis, and they can deliver several functional food
products to the market.
Methods of Extraction of Antioxidants
Extraction is a separation process used for separating solutes, i.e.
bioactive constituents from solutions using specific solvents by
adopting standard procedures (Handa et al., 2008). The main pur-
pose of this extraction method is to separate the soluble solutes
from the plant by-products for performing the efficient extraction
process. The crude extracts obtained by using these methods con-
tain complex mixtures of several plant metabolites viz. alkaloids,
glycosides, phenolics, terpenoids, and flavonoids. These extracts are
quiet being used as a medicinal agent in the form of tinctures and
fluid extracts. There are several methods that are available to effi-
ciently extract antioxidants from plant by-products of processing
industries, and these methods are discussed with their commercial
applications.
Conventional extraction techniques
Classical/conventional extraction techniques are being used at a
small scale level to extract bioactive components from several plant
materials. These techniques are usually based on the extraction effi-
ciency of different solvents, which are being used for this purpose. It

Table 1.  Amount of by-products generated from fruit and vegetable processing industry.

Fruit/vegetable By-products Edible part Reference

Agave 40% (rind and pith) 60% Iniguez-Covarrubias et al. (2001)

Apple 11% (pulp and seed core) 89% Ayala-Zavala et al. (2010)
Artichoke Around 60% (outer bracts, receptacles, and stems) 40% Llorach et al. (2002)
Asparagus Up to 40%–50% (spear) 50%–60% Rodriguez et al. (2006)
Banana Up to 30% (peel) 70% Schieber et al. (2001)
Cactus pear cladodes 20% (spines, glochids, and peel) 80% Bensadon et al. (2010)
Cactus pear fruit 45% (spines, glochids, peel, and unusable pulp) 65% Bensadon et al. (2010)
Carrot 30%–40% (pomace) 60%–70% Schieber et al. (2001)
Cyphomandra betacea 15%–35% (skin, pulp, and seeds) 65%–85% Ordonez et al. (2010)
Guava 10%–15% (peel and seeds) 85%–90% Schieber et al. (2001)
Mandarin 16% (peels) 84% Ayala-Zavala et al. (2010)
Mango 13.5% (seeds), 11% (peels), and 17.9% (unusable pulp) 58% Ayala-Zavala et al. (2010)
Orange 66% (peel) 44% Li et al. (2006)
Papaya 6.5% (seeds), 8.5% (peels), and 32.1% (unusable pulp) 53% Ayala-Zavala et al. (2010)
Passion fruit >75% (rind and seeds) 25% Schieber et al. (2001)
Pineapple 9.1% (core), 13.5% (peels), 14.9% (top), and 14.5% (pulp) 48% Ayala-Zavala et al. (2010)
Potato 15%–40% (peel) 60%–85% Schieber et al. (2001)
Tomato 3%–7% (peel and seeds) 93%–97% Schieber et al. (2001)
Tiger nuts (‘Chufa’) Up to 60% (solid and liquid wastes) 40% Sanchez-Zapata et al. (2009)
Recent advances in extraction of antioxidants, 2017, Vol. 1, No. 1
is a three-process approach, which consists of 1. soxhlet extraction,
2. maceration, and 3. hydrodistillation (HD).
The soxhlet extraction technique has been widely used for
extracting several bioactive compounds from various plant materi-
als. Dry plant material sample needs to be kept in the thimble. The
thimble is then placed in the distillation flask, which contains selec-
tive solvent when overflow level of solvent is reached; the solution of
the thimble-holder is aspirated by a siphon. Siphon unloads the solu-
tion back into the distillation flask. This solution carries extracted
solutes into the bulk liquid. Solute is remained in the distillation
flask and solvent passes back to the solid bed of plant. The process
runs repeatedly until the extraction is completed.
Maceration step was used at homemade level for preparing tonic
since from olden days. This becomes popular and also one of the
cheapest ways to obtain several essential oils and bioactive com-
pounds from different plant materials. For smaller scale of extrac-
tion, maceration process generally consists of several steps. First,
the materials are ground, i.e. their size is being reduced in order to
increase the surface area for uniform mixing with chosen solvent.
As a second step, in maceration process, appropriate solvent, i.e.
menstruum, is added in a closed vessel. Third, the liquid is strained
off but the marc, which is the solid residue of this extraction pro-
cess is pressed to recover large amount of occluded solutions. The
obtained strained and the press out liquid are mixed and separated
from impurities by filtration.
Occasional shaking in maceration process will facilitate extrac-
tion by means of two ways: at first, it will increase diffusion and
second, it will remove concentrated solution from the sample sur-
face for bringing new solvent to the menstruum for achieving more
extraction yield. HD, which is one of the traditional method used
for extracting bioactive compounds and essential oils from several
plant materials. In this process, organic solvents are not involved,
and it can be performed before dehydration of any plant materials.
There are three types of HD: water distillation, water and steam
distillation, and direct steam distillation (Vankar, 2004). In HD,
first, the plant materials are packed in a still compartment; sec-
ond, water is added in sufficient amount and then brought to boil.
Alternatively, direct steam is also injected into the plant sample.
Both hot water and steam can act as the main influential factors for
releasing bioactive compounds from several plant tissues. Indirect
cooling by water condenses the vapour mixture of water and oil.
Condensed mixture flows from condenser to a separator, where oil
and bioactive compounds were separated automatically from the
water (Silva et al., 2005). HD involves three main physicochemi-
cal processes: 1. hydrodiffusion, 2. hydrolysis, and 3. decomposi-
tion by heat. At higher extraction temperature, some of the volatile
components will be lost. Therefore, this drawback limits its use
Table 2.  Example of some extracted bioactive compounds by different solvents.
Water (1.000) Ethanol (0.654) Methanol (0.762)
Anthocyanins Tannins Anthocyanin
Tannins Polyphenols Terpenoids
Saponins Flavonol Saponins
Terpenoids Terpenoids
Alkaloids
Values in brackets indicates the relative polarity of each solvents. The values for relative polarity are normalized from measurements of solvent shifts of absorp-
tion spectra and were extracted from Reichardt (2003).
Source: Adapted from Cowan (1999).
63
for extraction of various thermolabile compounds from different
plant tissues.
The extraction rate of any conventional method mainly depends
on the choice of using selective solvents (Cowan, 1999). Table  2
shows the examples of various bioactive compounds, which are
being extracted by using different solvents. The solvent polarity is
one of the most important factors for the targeted compound, and
while selecting the solvent, the molecular affinity between chosen
solvent and solute, its environmental safety, toxicity, and its eco-
nomic feasibility needs to be considered to a higher extent for effi-
cient extraction of antioxidants.
Non-conventional extraction techniques
The major challenges of conventional extraction are longer extrac-
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tion time, requirement of costly and high purity solvent, evapo-
ration of the huge amount of solvent, low extraction selectivity,
and thermal decomposition of thermolabile compounds (Luque-
de-Castro and Garcia-Ayuso, 1998). To overcome these limitations
of conventional extraction methods, new and promising extrac-
tion techniques are introduced. These techniques are referred as
non-conventional extraction techniques. Some of the most prom-
ising techniques are ultrasound-assisted extraction (UAE), pulsed
electric field (PEF) extraction, enzyme-assisted extraction (EAE),
microwave-assisted extraction (MAE), pressurized liquid extrac-
tion (PLE), supercritical fluid extraction (SFE), pressurized low-
polarity water extraction, and molecular distillation. Some of these
techniques are considered as ‘green techniques’ as they comply
with standards set by Environmental Protection Agency (2015).
These include less hazardous chemical synthesis; designing safer
chemicals, safe solvents auxiliaries, design for energy efficiency,
use of renewable feedstock, reduce derivatives, catalysis, design to
prevent degradation, atom economy, and time analysis for pollu-
tion prevention and inherently safer chemistry for the prevention
of accident.
Ultrasound-assisted extraction
Ultrasound is a special type of sound wave beyond human hear-
ing, and its frequency ranges from 20 kHz to 100 MHz. Like other
waves, it can pass through a medium by creating compression and
expansion. Therefore, this process produces a phenomenon known
as cavitation, which further leads in production, growth, and col-
lapse of bubbles. A large amount of energy can be produced during
the conversion of kinetic energy of motion, and thereby, it helps in
heating the contents of the bubble (Herrera and Luque-de-Castro,
2004). According to Suslick and Doktycz (1990), bubbles have
temperature about 5000  K, pressure of 1000 atmosphere, heating,
Chloroform (0.259) Ether (0.117) Acetone (0.355)
Terpenoids Alkaloids Flavonoids
Flavonoids Terpenoids
Tannins
Flavones
Polyphenols
Anthocyanin
64
and cooling rate above 1010 K/s. Based on this principle, UAE has
been developed. Only liquid and liquid containing solid materials
have cavitation effect. The intensification of extraction process using
ultrasound has been attributed to the cavitation phenomena. The
effects caused by the ultrasonic waves are compression and expan-
sion cycles during the passage through the fluid. The expansion can
create bubbles or cavities in a liquid. This is so when the negative
pressure exerted, which exceeds the local tensile strength of the liq-
uid, may varies depending on its nature and purity. The process by
which vapour bubbles form, grow, and undergo implosive collapse is
known as cavitation. The conditions within these imploding bubbles
can be dramatic, with temperatures of 4500°C and pressures up to
100 MPa, which in turn produces very high shear energy waves and
turbulence in the cavitation zone. The combination of these factors
(pressure, heat, and turbulence) is used to accelerate mass transfer in
the extraction process (Patist and Bates, 2008).
The extraction mechanism by ultrasound process involves two
main types of physical phenomena: 1. the diffusion across the cell
wall and 2.  rinsing the contents of cell after breaking the walls
(Mason et al., 1996). Moisture content of sample, milling degree,
particle size, and solvent are very important factors for obtaining
efficient and effective extraction. Furthermore, temperature, pres-
sure, frequency, and time of sonication were the governing factors
for the action of ultrasound. UAE have also been incorporated
along with various classical techniques as they are reported to
enhance the efficiency of a conventional system. In a solvent extrac-
tion unit, an ultrasound device is placed in an appropriate position
to enhance the extraction efficiency (Vinatoru et  al., 1998). The
advantages of UAE include reduction in extraction time, energy,
and use of solvent. Ultrasound energy for extraction also facili-
tates more effective mixing, faster energy transfer, reduced thermal
gradients and extraction temperature, selective extraction, reduced
equipment size, faster response to process extraction control, quick
start-up, increased production, and it eliminates process steps
(Chemat et al., 2008).
UAE is seemed to be an effective extraction technique for bio-
active compound extraction from by-products of fruit and veg-
etable processing industries. Herrera and Luque-de-Castro (2004)
extracted phenolic compounds such as rutin, naringin, naringenin,
quercetin, ellagic acid, and kaempferol from strawberries using 0.8-s
duty cycle for 30 s by developing semi-automatic method based on
ultrasounds. Anthocyanins and phenolic compounds were extracted
from grape peel using UAE, and the extraction process was opti-
mized with reference to solvent, extraction temperature, and time
(Ghafoor et  al., 2009, 2011). In a study conducted by Cho et  al.
(2006), the impact of UAE on resveratrol recovery from grapes was
evaluated. With UAE, they obtained a significant resveratrol yield
(up to 24 and 28% in Campbell and Gerbong grape, respectively)
and a decrease of the extraction time compared to traditional solvent
extraction at 60°C for 30 min. Moreover, El-Darra et al. (2013) also
obtained a significant increase (up to 7%) in polyphenols (anthocya-
nins and tannins content) recovery, colour intensity, and scavenging
activity in the extracts obtained after applying ultrasound treatments
(USN) (24 kHz, 5–15 min, 121–363 kJ/kg) during red fermentation
of Cabernet Franc grapes.
Corrales et al. (2008b) studied the effects of UAE combined with
thermal treatment (70°C) to recover antioxidant bioactive com-
pounds from grape by-products. They observed a significant increase
in total phenolic compounds of the extracts obtained after apply-
ing USN treatments compared to conventional water extraction.
M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1
Similarly, Vilkhu et  al. (2008) obtained a significant improvement
in polyphenols extraction yield (6–35%) when they applied UAE in
red grape marc. Recently, Da-Porto et al. (2013) studied the perfor-
mance of conventional solvent extraction (Soxhlet) and ultrasounds
on grape seed oil extractions.
On the other hand, the effects of USN (1010 kJ/kg) on the recov-
ery of proteins and polyphenols from vine shoots was evaluated, and
a significant increase in the extraction of polyphenols was obtained
(Rajha et al., 2014). However, the energy consumption to reach simi-
lar levels of recovered polyphenols was incredibly higher compared
to other alternative physical treatments such as high-voltage elec-
trical discharges (HVED) (10 kJ/kg) and PEF (50 kJ/kg). The UAE
method was used to optimize the extraction of phenolic compounds
from pumpkins and peaches (Altemimi et al., 2016). Lu et al. (2015)
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optimized the UAE conditions using Box-Behnken design and evalu-
ated the antioxidant activity of total flavonoids from Cryptotaenia
japonica Hassk. Their results indicated that UAE is a promising tech-
nique for extraction of flavonoids from C. japonica Hassk, and the
flavonoids could be explored as a potential antioxidant agent for use
in medicine or functional foods.
Process system.  UAE experiments can be performed with a sonotrode
and a glass reaction tank (Hielsher, 2013). The double-layered mantle
of the reactor, which allows the control of extraction temperature with
a cooling system by means of water circulation. The transducer is
connected to the horn with a ‘booster’ installed in amplification mode
and finally the sonotrode, which needs to be immersed into the mid-
dle of the liquid and samples have to be filled in the tank (Figure 1).
Continuous UAE is carried out with an apparatus (Figure 2), which
is made up of a circulatory pump and the inlet is placed in a large
beaker, which contains water and samples (Del-Valle et al., 2005).
Industrial applications.  The interest of UAE lies in the reduced cost
due to decrease in time of extraction, a more effective and focused use
of power, a better yield, and more concentrated extract at compara-
ble S/L (solid–liquid) ratio. Conventional maceration process, which
is quiet time- and energy-consuming process, cannot be adopted at
commercial level for efficient extraction of antioxidants. The extrac-
tion process takes a reasonable amount of time (30 min); therefore, it
is possible for the conversion of the batch system towards a continu-
ous system. An experimental pilot study was carried out in a con-
tinuous piston apparatus for extraction of antioxidants from boldo
leaves (Petigny et al., 2013). From their lab study, they reported that
the selected conditions for the ultrasound extraction pilot study were
at the optimum conditions of temperature (36°C) and of ultrasound
density of power (23 W/cm2). They found that the 30-min time are
required to perform an effective and relevant extraction of soluble
material, which are similar to a conventional maceration process;
therefore, this time of extraction is further optimized for continuous
extraction of antioxidants. They also found that the yield of solu-
ble material from the ultrasound extraction pilot device was equal
to batch UAE process at equal time of extraction (21.7% yield of
extraction). Their result showed that the potential use of ultrasound
extraction was promising for extraction of antioxidants on an indus-
trial scale. They concluded that this process can be considered as a
sustainable alternative for the industries, since it allows simplified
handling, time reduction, quantity of targeted extracts improved,
and indicating the potential for the use of ultrasound extraction on
an industrial scale.
Recent advances in extraction of antioxidants, 2017, Vol. 1, No. 1
Figure 1.  Batch ultrasonic-assisted extraction (modified from Petigny et al., 2013).
Figure 2.  Ultrasonic pilot continuous extraction (modified from Petigny et al., 2013).
Pulsed electric field extraction
The PEF extraction method was one of the well-known technique
for improving the drying, extraction, and diffusion processes since
last decade (Barsotti and Cheftel, 1998; Angersbach et  al., 2000;
Vorobiev et  al., 2005; Vorobiev and Lebovka, 2006). The main
principle of PEF extraction is to disintegrate the structure of cell
membrane for increasing the rate of extraction. The electric poten-
tial passes through the cell membrane when it is suspended in an
electric field, and this electric potential separates membrane mol-
ecules based on dipole nature, i.e. according to their charge in the
cell membrane. After exceeding a critical value of approximately 1 V
of transmembrane potential, there is a repulsion, which may occurs
between the charge carrying molecules that form pores in weak areas
65
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of the membrane, and therefore, it causes drastic increase in perme-
ability (Bryant and Wolfe, 1987). For PEF treatment of plant materi-
als, a simple circuit with exponential decay pulses is used. The plant
materials were placed in a treatment chamber, which consists of two
electrodes. Based on treatment chamber design, the PEF process can
be operated in either continuous or batch mode (Puertolas et  al.,
2010). The effectiveness of PEF treatment depends on the process
parameters, which includes field strength, specific energy input, pulse
number, treatment temperature, and properties of the materials to be
treated (Heinz et al., 2003).
PEF can increase mass transfer during extraction by destroy-
ing membrane structure of plant materials for achieving enhanced
extraction and thereby decreasing the extraction time. PEF has
66
been applied to improve release of intracellular compounds from
plant tissue with the help of increasing the cell membrane perme-
ability (Toepfl et  al., 2006). PEF treatment at a moderate electric
field (500 and 1000 V/cm; for 10–4 to 10–2  s), which is found to
damage cell membrane of plant tissue with a slight increase in tem-
perature (Fincan and Dejmek, 2002; Lebovka et al., 2002). The PEF
can minimize the degradation of heat sensitive compounds (Ade-
Omowaye et  al., 2001). It is also applicable on plant materials as
a pre-treatment process prior to conventional extraction method in
order to lower the extraction effort (Lopez et al., 2009). PEF treat-
ment at (1  kV/cm with low energy consumption of 7 kJ/kg) in a
solid–liquid extraction (SLE) process for extraction of betanin from
beetroots showed highest degree of extraction compared to freezing
and mechanical pressing (Fincan et al., 2004). Corrales et al. (2008b)
extracted bioactive compound such as anthocyanins from grape
by-product using various techniques and found better extraction
of anthocyanin monoglucosides by PEF. The application of a PEF
treatment on grape skin before maceration step can reduce the dura-
tion of maceration and improve the stability of bioactives (antho-
cyanin and polyphenols) during vinification (Lopez et  al., 2008).
The permeabilization of Merlot skin by a PEF treatment resulted
in increased extraction of polyphenols and anthocyanins (Delsart
et al., 2012). For example, in the case of grape skins, Boussetta et al.
(2009, 2015) have shown that both PEF and HVED treatments had
a positive effect on the extraction of polyphenols and total solutes
from Chardonnay grape skins. The amount of polyphenol extracts
was significantly higher immediately after HVED treatment (40 kJ/
kg) (a four times increase as compared to a control extraction) and
then reached a maximum. After application of PEF treatment (1300
V/cm, 200 kJ/kg), the polyphenol content was also increased twice.
The initial extraction rates were also different for control extrac-
tion and PEF or HVED assisted extraction, but the final amounts of
polyphenols remains the same after 3 h of extraction process. Bouras
et al. (2016) studied the aqueous solid/liquid extraction of the poly-
phenols contained in Norway spruce [Picea abies (L.) Karst.] bark
by using PEF treatment. The feasibility of PEF treatment was studied
through two different PEF protocols with an intensity of E = 20 kV/
cm. These two PEF protocols are applied at different initial humidity
of the bark samples (14 and 21%). PEF treatments protocols were
Figure 3.  Components of pulsed electric field treatment and flow chart of process (modified from Gamli, 2014).
M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1
compared to untreated samples (simple diffusion without PEF) and
to diffusion from sawdust of Norway spruce bark. The results of
their study showed the positive effect of the PEFs on intracellular
compounds extraction. The PEF treatment also enhanced extrac-
tion of total phenolic content and antioxidant activity. They found
that the total phenols content was drastically increased to more than
eight times as a result of using PEF treatment.
Process system.  The PEF system consists of high current generator,
treatment unit, fluid handling system, and controlling equipments.
The generator of high current supplies electrical pulses of volt-
ages, shapes, and application time by using pulse-forming systems.
The system consists of power supplier, charging resistor, capacitor,
switches, inductors, and resistors. Power generator converts high-
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voltage (50–60 Hz frequency) alternating current (AC) power to the
high direct current power (DC). The energy produced by the gen-
erator (5–80  kV DC) is stored at capacitors and used to generate
electric fields.
Systems have a switch that is used to discharge high energy through
the food materials in treatment chamber. Switching systems are the
elements that connect storage device (capacitors) and energy load at
treatment chamber. The switch determines necessary pulse current
and application time. It acts as a bridge between high-energy suppliers
and treatment unit (Mohammed and Ayman, 2012; Vallverdu-Queralt
et al., 2013). It is reported that many different waveforms are being
applied in PEF treatment. Pulse shapes are commonly being used with
either exponentially or square wave. Square wave producing systems
require a switch with turn off capability or pulse-forming network
(Toepfl et al., 2007). The PEFs generated by a generator are used in
treatment unit or chamber. Treatment units are designed to operate
either batch or continuous manner. The components of PEF treatment
and flow chart of process are given in Figure 3. Semi-liquid or liquid
food materials are pumped to the treatment chamber at a certain flow
rate (5–100 ml/min) within co-axial or parallel plate types in chamber
(Pizzichemi, 2007). The flow of parallel type is being used for batch
system, while co-axial flow systems are used for continuous types. In
both systems, liquid and semi-liquid materials are being pumped at
a certain flow rate, and the PEFs are applied at any pulse frequency.
It is reported that treatment chamber should consist of parallel plate
Recent advances in extraction of antioxidants, 2017, Vol. 1, No. 1
electrodes and space insulator. The electrodes are separated from the
fluid materials by ion conductive membranes that are made up of
sulfonated polystyrene and acrylic acid copolymers, and electrolyte
is being used to simplify electrical conduction between the electrodes
and membranes (Dunn and Pearlman, 1987).
Industrial applications. PEF technology is most widely used in
the food processing industries. In the 1980s, the Krupp (German
equipment manufacturer) has performed first attempts to com-
mercialize the process, but at this time, pulsed power switches
have not shown sufficient performance and reliability (Sitzmann
and Munch, 1988; Sitzmann, 2006, personal communication). In
the 1990s, in the USA as well as Europe, various food processors,
equipment manufacturers, and universities have been formed to
develop PEF applications and equipment (Toepfl et  al., 2006). In
1995, a continuous system was launched by PurePulse, a subsidi-
ary of Maxwell Laboratories. In 2006, a first commercial instal-
lation for fruit juice preservation was achieved in the USA, but
it was stopped in 2008 due to technical and commercial limita-
tions. The first commercial operation in Europe was achieved in
2009, with the installation of a 1500 l/h juice preservation line. In
2010, the first industrial system for processing of vegetables with
a maximum capacity of 50 t/h was started. At present, such PEF-
treated food products were commercially available in countries viz.
Netherlands, Germany, and UK, where PEF-processing equipment
with a capacity of 1500–2000 and 5000–8000 l/h is used (Irving,
2012; Mchugh and Toepfl, 2016). An industrial system to enhance
yield of cloudy apple juice is operated in a German fruit juice com-
pany in a 10 t/h scale (Muller et al., 2007). Textural changes was
observed in potato, sugar beet, and carrot after an PEF treatment,
as a result of facilitation of handling, pumping, or cutting processes
(Lebovka et  al., 2004; Janositz and Knorr, 2010). The process is
currently being used with a several industrial installations in order
to replace conventional pre-heating of potatoes (60°C, 30 min) in
French fries production process (Mchugh and Toepfl, 2016).
Enzyme-assisted extraction
Some phytochemicals in the plant matrices are dispersed in cell
cytoplasm, and some compounds are retained in the polysaccharide-
lignin network by hydrogen bonding or hydrophobic interactions,
which are not accessible with a solvent in a routine extraction pro-
cess. Enzymatic pre-treatment has been considered as a novel and
an effective way to release bounded compounds and also to increase
overall yield (Rosenthal et  al., 1996). The addition of specific
enzymes such as cellulase, α-amylase, and pectinase during extrac-
tion enhances recovery by breaking the cell wall and hydrolyzing the
Figure 4.  The process of enzyme-assisted extraction method from the natural products (modified from Cheng et al., 2015).
67
structural polysaccharides and lipid bodies (Rosenthal et al., 1996;
Singh et al., 1999).
Extraction process. There are two approaches for EAE process:
1.  enzyme-assisted aqueous extraction (EAAE) and 2.  enzyme-
assisted cold pressing (EACP) (Latif and Anwar, 2009). Usually,
EAAE methods have been developed mainly for the extraction of
oils from various seeds (Rosenthal et al., 1996; Hanmoungjai et al.,
2001; Rosenthal et al., 2001; Sharma et al., 2002). In EACP tech-
nique, enzymes is used to hydrolyze the seed cell wall because in this
system polysaccharide-protein colloid is not available, which is obvi-
ous in EAAE (Concha et al., 2004). Various factors including enzyme
composition and concentration, particle size of plant materials, solid
to water ratio, and hydrolysis time are recognized as key factors for
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extraction (Niranjan and Hanmoungjai, 2004). Dominguez et  al.
(1995) reported that the moisture content of plant materials is also
an important factor for enzymatic hydrolysis.
The process of EAE method from the natural products was
shown in Figure 4. The breakdown of cell walls is the critical step
for the extraction of many bioactive compounds, which are existing
inside the cell walls. EAE is based on the ability of enzymes to hydro-
lyze cell wall components and disrupt the structural integrity of the
plant cell wall under mild process conditions, thereby allowing the
efficient extraction and release of the bioactive compounds (Pinelo
et al., 2006; Gardossi et al., 2010). There is a direct proportionality
between the rate and the substrate concentration until the enzyme
concentration becomes limited (Sowbhagya and Chitra, 2010). In
this process, several parameters need to be considered for efficient
extraction process, which includes temperature of reaction, time of
extraction, pH of system, enzyme concentration, and particle size of
substrate.
Bhattacharjee et al. (2006) described EACP as an ideal alternate
for extracting bioactive components from oilseed because of its non-
toxic and non-inflammable properties. The oil extracted by enzyme-
assisted methods was found to contain higher amount of free fatty
acids and phosphorus contents than traditional hexane extracted oil
(Dominguez et  al., 1995). The EAAE is recognized as eco-friendly
technology for extraction of bioactive compounds from oil because
it uses water as solvent instead of organic chemicals (Puri et  al.,
2012).
EAAE of phenolic antioxidants from grape pomace during wine
production was tested by Meyer et  al. (1998), who found a cor-
relation between yield of total phenols and degree of plant cell wall
breakdown by enzyme. Landbo and Meyer (2001) showed improved
release of phenolic compounds from Ribes nigrum pomace using var-
ious enzymes. Li et al. (2006) extracted total phenolic contents from
68
five citrus peels (Yen Ben lemon, Meyer lemon, grapefruit, manda-
rin, and orange) by EAAE using different enzymes, and the recovery
was highest with celluzyme MX. Maier et al. (2008) used mixture
of pectinolytic and cellulolytic enzyme in the ratio of 2:1 to extract
bioactive compounds (phenolic acids, non-anthocyanin flavonoids,
and anthocyanins) from grape pomace, where obtained yields were
higher compared with sulfite-assisted extraction. Extraction of phe-
nolic antioxidant from raspberry solid wastes was increased by
application of enzyme in hydro-alcoholic extraction compared with
non-enzymatic control (Laroze et  al., 2010). Gomez-Garcia et  al.
(2012) extracted phenolic compounds from grape waste using dif-
ferent types of enzymes viz. celluclast, pectinex, and novoferm in
EAAE and found that novoferm had the strongest effect on phenolic
release from grape waste.
Ranveer et al. (2013) conducted the study in order to optimize the
extraction process of lycopene by using solvents and also to exam-
ine the effect of enzyme treatment on the recovery of lycopene. The
extraction of lycopene was carried out with four different solvents
to know their extraction efficiency. Two-step extraction processes
was followed for EAE of lycopene. In the first step, waste samples
were treated with enzymes, i.e. cellulase and pectinase, where as in
second step, extraction of lycopene was carried out by using sol-
vent. Enzyme-assisted solvent extraction of phenolic compounds
from watermelon (Citrullus lanatus) rind was optimized (Mushtaq
et al., 2015). The results obtained indicated that optimized enzyme-
assisted solvent extraction enhanced the liberation of antioxidant
phenolics up to 3-folds on fresh weight basis as compared to con-
ventional solvent extraction, with substantial level of total phenolics.
Industrial applications.  The EAE method has several technical limita-
tions when it is being commercially adopted (Puri et al., 2012). The
enzymes used for extraction is quiet expensive for large-scale industrial
production process. Certain enzymes cannot breakdown the plant cell
walls completely. Therefore, the EAE is not always feasible method to
be applied on industrial scale basis because enzymes behaviour was
limited by environmental conditions rigidly, and the above limitations
were needed to be considered in order to make full use of enzymes of
potential value in the exploitation and utilization of natural products.
Microwave-assisted extraction
The MAE is also considered as a novel method for extracting soluble
products into a fluid from a wide range of materials using microwave
Table 3.  Critical properties of commonly used supercritical fluids.
Fluid Molecular weight (g/mol)
Carbon dioxide 44.01
Water 18.02
Methane 16.04
Ethane 30.07
Propane 44.09
Ethylene 28.05
Propylene 42.08
Methanol 32.04
Ethanol 46.07
Acetone 58.08
Ammonia 17.031
Chlorotrifluoromethane 104.46
Diethyl ether 74.12
n-Pentane 72.15
Source: Adapted from Liong et al. (1991).
M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1
energy (Pare et  al., 1994). Microwaves are electromagnetic fields in
the frequency range from 300 MHz to 300 GHz. They are made up of
two oscillating fields that are perpendicular such as electric field and
magnetic field. The principle of heating using microwave is based on
its direct impacts on polar materials (Letellier and Budzinski, 1999).
Electromagnetic energy is converted to heat following ionic conduc-
tion and dipole rotation mechanisms (Jain, 2009). During ionic con-
duction mechanism, heat is generated because of the resistance of
medium to flow ion. On the other hand, ions keep their direction along
field signs, which change frequently. This frequent change of direc-
tions results in collision between molecules and consequently gener-
ates heat. The larger the dielectric constant of the solvent (Table 3),
the more optimal the heating (Kaufmann and Christen, 2002). In the
case of extraction, the advantage of microwave heating is the disrup-
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tion of weak hydrogen bounds promoted by the dipole rotation of the
molecules. A higher viscosity of the medium lowers this mechanism by
affecting molecular rotation. The migration of dissolved ions increases
solvent penetration into the matrix and thus facilitates the solvation
of the analyte (Kaufmann and Christen, 2002). The extraction mecha-
nism of MAE is supposed to involve three sequential steps described
by Alupului et al. (2012): first, separation of solutes from active sites
of sample matrix under increased temperature and pressure; second,
diffusion of solvent across sample matrix; third, release of solutes
from sample matrix to solvent. Several advantages of MAE have been
described by Cravottoa et al. (2008) such as quicker heating for the
extraction of bioactive substances from plant materials; reduced ther-
mal gradients; reduced equipment size; and increased extract yield.
MAE can extract bioactive compounds more rapidly, and a better
recovery is possible than conventional extraction processes. MAE is
also recognized as a green technology because it reduces the use of
organic solvent (Alupului et al., 2012).
Dhobi et  al. (2009) showed increased extraction efficiency of
MAE by extracting a flavolignin, silybinin from Silybum mari-
anum compared with the conventional extraction techniques such
as soxhlet and maceration. Asghari et  al. (2011) extracted some
bioactive compounds (E- and Z-guggolsterone, cinnamaldehyde,
and tannin) from various plants under optimum conditions and
showed that MAE is a faster and easier method in comparison
to conventional extraction processes. MAE process from Chinese
quince (Chaenomeles sinensis) was optimized for solvent concen-
tration, extraction time, and microwave power using designed
experiments to maximize recoveries of flavonoids and phenolics
Critical temperature (K) Critical pressure (MPa)
304.1 7.38
647.3 22.12
190.4 4.60
305.3 4.87
369.8 4.25
282.4 5.04
364.9 4.60
512.6 8.09
513.9 6.14
508.1 4.70
405.6 11.3
302 3.92
467.7 3.64
469.6 3.37
Recent advances in extraction of antioxidants, 2017, Vol. 1, No. 1
and also to enhance electron donating ability of the extracts (Hui
et al., 2009). Liazid et al. (2011) studied the MAE of anthocyanins
from grape skins. Bittar et al. (2013) produced grape juice rich in
polyphenols by MAE. Yu et al. (2014) performed both single-factor
and orthogonal experiments to evaluate different MAE processing
conditions for polyphenol extraction from grape skin. MAE was
employed to extract silymarin from milk thistle seeds (Zheng et al.,
2009). MAE method was applied successfully to extract silymarin
from milk thistle seeds. Thirugnanasambandham and Sivakumar
(2017) optimized the operating parameters in MAE process such
as temperature, mass of the sample, extraction time on the betalain
content from dragon fruit peel using response surface methodol-
ogy. Wild apple fruit dust, discarded as by-product from filter tea
factory, which represents one of the underutilized raw material,
which found to contain high amount of bioactive compounds.
Therefore, Pavlic et al. (in press) utilized the wild apple fruit dust
for recovery of polyphenolic antioxidants by application of MAE
process. Results showed that wild apple fruit dust could be used as
good source for recovery of polyphenols and preparation of liquid
extracts with increased antioxidant activity.
Process  system.  The MAE systems are classified into multi-mode
system and focused-mode system (mono-mode). Multi-mode system
allows random dispersion of microwave radiation in cavity by a mode
stirrer, while focused system (mono-mode) allows focused microwave
radiation on a restricted zone in cavity. Usually, the multi-mode system
is associated with high pressure (HP), while the mono-mode system
is employed under atmospheric operating pressure. However, mono-
mode system can also run at HP. In order to avoid confusion in the
classification of MAE, ‘Closed System’ and ‘Open System’ are gener-
ally used to refer to the system that operates above atmospheric pres-
sure and under atmospheric pressure, respectively (Dean and Xiong,
2000; Garcia and Castro, 2003). The schematic diagrams of closed
system and open system are illustrated in Figure 5a and 5b.
In a closed MAE system, the extractions are carried out in
a sealed vessel with different mode of microwave radiations.
Extraction is normally carried out under uniform microwave heat-
ing. High working pressure and temperature of the system allow
fast and efficient extraction. The pressure inside the extraction ves-
sel is controlled in such a way that it would not exceed the working
pressure of the vessel, while the temperature can be regulated above
the normal boiling point of the extraction solvent. Recent advance-
ments in the closed system have led to the development of high-
pressure MAE. The increase in temperature and pressure accelerates
MAE due to the ability of extraction solvent to absorb microwave
Figure 5.  (a) Closed type microwave system and (b) open type microwave system (modified from Mandal et al., 2007).
69
energy (Wang et al., 2008). Despite the fact that the closed system
offers fast and efficient extraction with less solvent consumption,
but it is susceptible to losses of volatile compounds with limited
sample throughput.
Open system is developed to counter the shortcomings of closed
system such as the safety issues, and it is considered more suitable for
extracting thermolabile compounds. This system has higher sample
throughput, and more solvent can be added to the system at anytime
during the process. Basically, open system operates at more mild con-
ditions. Open MAE system is widely used in the extraction of active
compounds, and it is also used in analytical chemistry. This system
operates at atmospheric conditions, and only part of the vessel is
directly exposed to the propagation of microwave radiation (mono-
mode). The upper part of the vessel is connected to a reflux unit to
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condense any vapourized solvent. Besides that, multi-mode radiation
can also be employed in open MAE system with the reflux unit.
Industrial applications. Filly et  al. (2014) proposed solvent free
microwave extraction as a green method for the extraction of essen-
tial oil from aromatic herbs that are extensively used in the food
industry. This technique is a combination of microwave heating
and dry distillation performed at atmospheric pressure without any
added solvent or water. The isolation and concentration of volatile
compounds is performed in a single stage. In their work, they used
solvent free microwave extraction and a conventional technique, HD
(Clevenger apparatus) as comparative method for the extraction of
essential oil from rosemary (Rosmarinus officinalis L.). Microwave
extraction and separation has been used to increase the concentra-
tion of the extract, when compared to the conventional method with
the same solid/liquid ratio, which reduces the extraction time and
separate at the same time of volatile organic compounds from non-
volatile organic compounds of boldo leaves (Petigny et al., 2014).
Pressurized liquid extraction
PLE was first described by Richter et  al. (1996). This method is
now known by several names: pressurized fluid extraction, acceler-
ated fluid extraction, enhanced solvent extraction, subcritical water
extraction (SWE), and HP solvent extraction (Nieto et  al., 2010).
The concept of PLE is the application of HP to remain solvent liq-
uid beyond their normal boiling point. HP facilitates the extraction
process. Automation techniques are the main reason for the greater
development of PLE-based techniques along with the decreased
extraction time and solvents requirement.
PLE technique requires small amounts of solvents because of
the combination of HP and temperatures, which provides faster
70
extraction. The higher extraction temperature can promote higher
analyte solubility by increasing both solubility and mass transfer rate
and, also decrease the viscosity and surface tension of solvents, thus
improving extraction rate (Ibanez et al., 2012).
In comparison to the traditional soxhlet extraction, PLE was
found to dramatically decrease time consumption and solvent
use (Richter et al., 1996). Therefore, for extraction of polar com-
pounds, PLE which is considered as one of the potential alternative
technique to SFE process (Kaufmann and Christen, 2002). PLE
is also useful for the extraction of organic pollutants from envi-
ronmental matrices those are stable at high temperatures (Wang
and Weller, 2006). PLE has also been used for the extraction of
bioactive compounds from marine sponges (Ibanez et  al., 2012).
Applications of PLE technique for obtaining natural products are
frequently available in literature (Kaufmann and Christen, 2002).
Additionally, due to small amount of organic solvent use, PLE gets
broad recognition as a green extraction technique (Ibanez et  al.,
2012).
PLE has been successfully applied to extract bioactive compounds
from different plant materials. In consideration of yield, reproduc-
ibility, extraction time, and solvent consumption, PLE has been con-
sidered as an alternate to conventional methods due to faster process
and lower solvent use. Flavonoids extracted from spinach by PLE
using a mixture of ethanol and water (70:30) solvent at 50–150°C
were more effective than water solvent at 50–130°C (Howard and
Pandjaitan, 2008). Luthria (2008) showed temperature, pressure,
particle size, flush volume, static time, and solid-to-solvent ratio
parameters, which are having greater influence on the extraction of
phenolic compounds from parsley (Petroselinum crispum) flakes by
using PLE method.
Some studies have been conducted in order to evaluate the recov-
ery of polyphenols from grape pomace and grape skin assisted by
HP (200–600 MPa, 20–70°C, 30–90 min) (Corrales et al., 2008a,
2008b, 2009). All of them obtained a significant increase in the
total and individual anthocyanin content after HP processing com-
pared to conventional extraction methods. On the other hand, the
potential of HP high temperature (HPHT) to extract phenolic com-
pounds from grape by-products (Casazza et al., 2010, 2012), and
particularly, resveratrol from grape skins was evaluated, obtaining
promising results. The research group investigated the extraction
efficiencies of phenolic compounds from grape seeds and skins
using numerous non-conventional versus traditional SLE methods.
Extraction yields and antioxidant activities were compared between
extracts obtained using SLE and non-conventional methods (UAE,
MAE, and HPHT). They found that ethanol was the preferred sol-
vent when compared to methanol for both skin and seed extrac-
tions. They concluded that by using HPHT process, high content
of total polyphenols, o-diphenols, and flavonoids in seeds and skins
was achieved.
Casazza et  al. (2012) investigated the potential use of HPHT
to recover phenolic compounds from grape skins. The authors
concluded that using HPHT technology resulted in enriched poly-
phenol extracts with high antiradical power. The grape marc was
subjected to phenolic compounds extraction by using HP and tem-
perature extraction process. Further, extracted phenolic compounds
were encapsulated at 0.1% final concentration using a non-emul-
sion-based delivery system. This encapsulation, formulated with
natural ingredients (sunflower and palm oils) and a hydrophilic and
hydrophobic emulsifier under HP homogenization, enhanced the
dispersibility in aqueous solutions. Antioxidant activities of encap-
sulated and non-encapsulated phenolics were evaluated using in
M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1
vitro [ferric reducing antioxidant power (FRAP) and oxygen radical
absorbance capacity] and cellular antioxidant assays. An interest-
ing conclusion of this work was the significant increase in cellular
antioxidant activity for the encapsulated grape marc polyphenols
when compared to the non-encapsulated molecules, revealing the
potential of nano-emulsions in the biological membrane delivery
systems (Sessa et al., 2012).
PLE is an another extraction technique that can enhance extrac-
tion rates of bioactive compounds. PLE was used to extract anti-
oxidants and polyphenols from industrially generated apple pomace.
A lower temperature range between 75 and 125°C is recommended.
Using this temperature range, a maximum antioxidant activity was
determined at 60% ethanol and 102°C. By using PLE, the antioxi-
dant activity was increased 2.4 times in comparison to traditional
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SLE, and the technique may be a promising alternative to conven-
tional techniques for extracting antioxidants. Saravana et al. (2016)
utilized PLE to extract sulfated polysaccharides (fucoidan) from
brown seaweed Saccharina japonica. They found that the best crude
fucoidan yield of 8.23% was obtained at 140°C temperature with
50 bar pressure. Shang et al. (2016) optimized the extraction meth-
ods for biological compound, i.e. tricin by PLE from black bamboo
leaves. The optimized extraction methods for biological compound
tricin by PLE from black bamboo leaves were obtained at 200°C,
50% ethanol, 20-min static time, and 425-μm particle size, achiev-
ing high extraction efficiency of 249-mg/100-g dry leaves. They con-
cluded that the high temperature is beneficial for extracting tricin
from black bamboo leaves.
Process  system.  The PLE set-up is shown in Figure  6. The solvent
was pumped into the extraction cell, which was placed in an electri-
cal heating jacket at a desired temperature, until the required pres-
sure was obtained. Extraction samples were placed in a 6.57  cm3
extraction cell containing a sintered metal filter at the bottom and
upper parts. The cell containing the sample was heated, filled with
extraction solvent, and then pressurized. The sample was placed
in the heating system for 5  min to ensure that the extraction cell
would be at the desired temperature (313–393  K) during the fill-
ing and pressurization procedure. After pressurization, the sample
with pressurized solvent was kept statically at the desired pressure
(5–10 MPa) for the desired time (3–15 min). After PLE, the extracts
were rapidly cooled to 5°C in ice water using amber flasks to prevent
anthocyanin degradation.
Industrial applications. Ko et  al. (2016) conducted a pilot-scale
SWE plant (8 l scale) for the scale-up and commercialization of the
SWE process that extracts antioxidant flavonoids from agricultural
by-products such as Citrus unshiu Markovich. The effects of oper-
ating parameters (extraction temperature, extraction time, material
type, solute/solvent ratio, and pressure) on the SWE of flavonoids
from dried satsuma mandarin peel were studied. From the practical
aspect, the optimum conditions for obtaining flavonoids by pilot-
scale SWE were as follows: extraction temperature of 130°C, extrac-
tion time of 15 min, and solute/solvent ratio of 1/34. The yields of
flavonoids obtained under laboratory and pilot conditions were sim-
ilar: 117.8 and 113.4 mg/g satsuma mandarin peel, respectively. The
proportion of flavonoids recovered by SWE in the pilot plant was
96.3%, and large-scale experiments using this method demonstrate
its potential industrial applications.
SWE is excellent technology to selectively extract flavonoids
using temperature-dependent dielectric constant properties of water.
Recent advances in extraction of antioxidants, 2017, Vol. 1, No. 1
Figure 6.  Pressurized liquid extraction set-up (modified from Santos et al., 2012).
Figure 7.  A symmetric diagram of SFE apparatus (modified from Yi et al., 2009).
Supercritical fluid extraction
The SFE technique has attracted wide scientific interest, and it was
successfully used in pharmaceutical, polymer, and food applications
(Zougagh et al., 2004). Several industries have been using this tech-
nique for many years, especially, decaffeinated coffee preparation
industries (Ndiomu and Simpson, 1988). Supercritical state is a dis-
tinctive state and can only be attained if a substance is subjected to
temperature and pressure beyond its critical point. Critical point is
defined as the characteristic temperature (Tc) and pressure (Pc) above
which distinctive gas and liquid phases do not exist (Inczedy et al.,
1998). In supercritical state, the specific properties of gas and/or
liquid changes, which means supercritical fluid cannot be liquefied
by modifying temperature and pressure. Supercritical fluid possesses
gas-like properties of diffusion, viscosity, and surface tension, and
liquid-like density and solvation power. These properties make it
71
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suitable for extracting compounds in a short time with higher yields
(Sihvonen et al., 1999). A basic SFE system consists of the following
parts: a tank of mobile phase, usually CO2, a pump to pressurize the
gas, co-solvent vessel and pump, an oven that contains the extraction
vessel, a controller to maintain the HP inside the system, and a trap-
ping vessel. Usually different type of meters such as flow meter, dry/
wet gas meter could be attached to the system. A symmetric diagram
of typical SFE instrumentation is given in Figure 7.
CO2 is considered as an ideal solvent for SFE. The critical
temperature of CO2 (31°C) is close to room temperature, and the
low critical pressure (74 bars) offers the possibility to operate at
moderate pressures, generally between 100 and 450 bar (Temelli
and Guclu-Ustundag, 2005). The main drawback of CO2 is its low
polarity, which makes it ideal for lipid, fat, and non-polar sub-
stance, but unsuitable for polar materials. The limitation of low
72
polarity of CO2 has been successfully overcome by the use of chemi-
cal modifier (Lang and Wai, 2001; Ghafoor et  al., 2010). Usually
a small amount of modifier is considered as useful to significantly
enhance the polarity of CO2. For example, 0.5 ml of dichlorometh-
ane (CH2Cl2) can enhance the extraction, which is same for 4-h HD
(Hawthorne et al., 1994).
The extraction of bioactive compounds from plant materials
relies upon several parameter of SFE, and most importantly, these
parameters are tunable (Raverchon and Marco, 2006; Raynie, 2006,
2010). The major variables influencing the extraction efficiency are
temperature, pressure, particle size, and moisture content of feed
material, time of extraction, flow rate of CO2, and solvent-to-feed
ratio (Temelli and Guclu-Ustundag, 2005; Ibanez et al., 2012). The
advantages of using supercritical fluids for the extraction of bioac-
tive compounds can be understood considering following points
(Lang and Wai, 2001): 1.  The supercritical fluid has a higher dif-
fusion coefficient and lower viscosity and surface tension than a
liquid solvent, leading to more penetration to sample matrix and
favourable mass transfer. Extraction time can be reduced substan-
tially by SFE when compared with conventional methods. 2.  The
repeated reflux of supercritical fluid to the sample provides complete
extraction. 3. The selectivity of supercritical fluid is higher than liq-
uid solvent as its solvation power can be tuned by changing either
temperature or pressure. 4. Separation of solute from solvent in con-
ventional extraction process can easily be by-passed by depressuriza-
tion of supercritical fluid, which will save time. 5. SFE is operated at
room temperature, so an ideal method for thermolabile compound
extraction. 6. In SFE, small amount of sample can be extracted com-
pared with solvent extraction methods. 7. SFE does not use organic
solvent and considered as environment friendly. 8. The recycling and
reuse of supercritical fluid is possible and thus minimizing waste
generation. 9.  SFE scale can be arranged on specific purpose from
few milligram samples in laboratory to tons of sample in industries.
10. SFE process provides information regarding extraction process
and mechanism, which can be manipulated to optimize extraction
process.
supercritical carbon dioxide (SC-CO2) modified with ethanol
(15% wt) gave higher extraction yields of naringin (flavonoid)
from citrus paradise than pure SC-CO2 at 9.5  MPa and 58.6°C
(Giannuzzo et  al., 2003). Polyphenols and procyanidins were
extracted from grape seeds using SFE, where methanol was used
as modifier and methanol modified CO2 (40%) released more than
79% of catechin and epicatechin from grape seed (Khorassani and
Taylor, 2004). Pascual-Marti et al. (2001) evaluated and optimized
the SFE conditions [pressure (80–110 bar), temperature (40°C),
ethanol concentration (5–15%), and extraction time (5–25 min)] to
recover resveratrol from grape skin of Vitis vinifera. They found that
the optimum SFE extraction conditions were obtained at 110 bar,
40°C, 7.5% ethanol, and extraction time of 15  min. Under these
conditions, the resveratrol content was totally recovered (100%). In
another study, the effect of SC-CO2 extraction (100–400 bar/35–
55°C) and the addition of modifier [5% (v/v) of ethanol] on the
recovery of resveratrol from grape seeds, stems, skin, and pomace of
the Palomino Fino grape variety were studied (Casas et al., 2010). It
was found that the maximum recovery of resveratrol was obtained
from skins (49.1 mg/100 g dry sample) when SC-CO2 was used at
400 bar/35°C and 5% (v/v) of ethanol as co-solvent.
Murga et al. (2000) evaluated the potential of mixtures of car-
bon dioxide and alcohol under supercritical conditions to selectively
extract phenolic compounds from grape seeds. Louli et  al. (2004)
studied the impact of a combined process of liquid and supercritical
M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1
solvent extraction to recover antioxidant compounds from winery
by-products. The authors studied the effect of solvent type, medium
composition (skins, seeds, stems), and crushing pre-treatment on the
antioxidant activity of the extract. They demonstrated that ethyl
acetate, used as solvent, provides the highest antioxidant activity of
extracts. Oliveira et al. (2013) investigated the antimicrobial activity
and the composition profile of the extracts obtained from Merlot
and Syrah grape pomace after applying SC-CO2 with co-solvent at
pressures up to 300 bar and temperatures of 50 and 60°C. Although
they found low extraction yields of polyphenols (gallic acid, p-OH-
benzoic acid, vanillic acid, and epicatechin), the obtained extracts
provided interesting antibacterial (Staphylococcus aureus, Bacillus
cereus, Escherichia coli, and Pseudomonas aeruginosa) and antifun-
gal (Candida albicans, Candida parapsilosis, and Candida krusei)
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activities. SFE is successfully and widely used for the extraction of
lycopene from ripe tomatoes (Cadoni et al., 2000) and tomato pro-
cessing wastes (Baysal et al., 2000; Kassama et al., 2008).
Farias-Campomanes et  al. (2015) utilized SFE method for
extraction of polyphenols from lees of pisco making (an alcoholic
beverage made from grapes by-products). SC-CO2 with 10% of eth-
anol (w/w) was used as extraction solvent. Overall extraction curves
were determined at 20 and 35 MPa, and the experimental data were
used to estimate the kinetic parameters. Conventional techniques
using ethanol as extraction solvent were performed for compara-
tive purposes. Their results show that the lower yield was obtained
when elevated pressures were used. They further observed from the
kinetic parameters that the mass transfer rate and the amount of
the extract dissolved in supercritical phase were found to be higher
at 20 MPa than 35 MPa. Polyphenols were rapidly extracted with
supercritical fluid, and more concentrated extracts were obtained
at 20 MPa. They concluded that the SFE at 20 MPa was the most
efficient technique for the extraction of polyphenols from lees of
pisco making.
Barbosa-Pereira et al. (2013) compared two methods of purify-
ing the crude extract solid-phase extraction (SPE) and SFE with the
aim of improving the quality of the final extract for potential use as
safe food additive, functional food ingredient, or nutraceutical. They
found that the predominant fractions yielded by SPE were the most
active, and the fraction eluted with 30% (v/v) of methanol displayed
the highest antioxidant activity (0.20 g/l). The most active fraction
yielded by SFE (EC50 of 0.23 g/l) was obtained under the follow-
ing conditions: temperature 40°C, pressure 140 bar, extraction time
30 min, ethanol (6%) as a modifier, and modifier flow 0.2 ml/min.
Finally, they concluded that SFE is the most suitable procedure for
purifying the crude extracts. Therefore, natural extracts obtained
from the residual stream and purified by SFE can be used as natural
antioxidants with potential applications in the food, cosmetic, and
pharmaceutical industries.
The pentacyclic triterpene α,β-amyrin is a promising bioactive
natural product. SFE and fractionation were used to obtain penta-
cyclic triterpene compounds from dried rosemary leaves (Bensebia
et al., 2016). Their results showed that the selective recovery of pen-
tacyclic triterpene can be optimized by adjusting the pressure and
temperature during the extraction process. They concluded that the
SFE technique as one of the excellent technique for effective extrac-
tion of pentacyclic triterpene α,β-amyrin from rosemary leaves.
SC-CO2 fluid technology
Process  system.  The SC-CO2 fluid extraction process is governed
by four key steps: extraction, expansion, separation, and solvent
Recent advances in extraction of antioxidants, 2017, Vol. 1, No. 1
conditioning. The steps are accompanied by four generic primary
components: extractor (HP vessel), pressure and temperature control
system, separator, and pressure intensifier. Raw materials are usually
ground and charged into a temperature-controlled extractor form-
ing a fixed bed, which is usually the case for a batch and single-stage
mode (Shi et al., 2007a, 2007c; Kassama et al., 2008).
The processes described above are semi-batch continuous processes
where the SC-CO2 flows in a continuous mode, while the extractable
solid feed is charged into the extraction vessel in batches. In commer-
cial scale processing plants, multiple extraction vessels are sequentially
used to enhance process performance and output. Although the system
is interrupted at the end of the extraction period, when the process
is switched to another vessel prepared for extraction, the unloading
and/or loading of the spent vessels can be carried out while extraction
is in progress, reducing the downtime, and improving the production
efficiency. A semi-continuous approach on a commercial scale uses a
multiple stage extraction processes that involve running the system
concurrently by harnessing a series of extraction vessels in tandem.
In this system, the process is not interrupted at the end of extraction
period for each vessel because the process is switched to the next pre-
pared vessel by control valves for extraction while unloading and/
or loading the spent vessels. Thus, SC-CO2 technology is available in
the form of single-stage batch that could be upgraded to multistage
semi-continuous batch operations coupled with a multi-separation
process. The need to improve the design into truly continuous modes
is growing. SC-CO2 fluid extraction could be cost-effective under large-
scale production. The effects of various parameters of SC-CO2 fluid
extractions of tomato skins on the extraction yields, and antioxidant
activities of lycopene-rich extracts were investigated (Yi et al., 2009).
The carotenoids in pumpkin were extracted by organic solvents and
by SC-CO2, and then, they were identified, quantified, and compared
(Kassama et al., 2008; Shi et al., 2010).
Industrial applications. Large-scale SC-CO2 fluid extraction has
become a practical process for the extraction of high-value prod-
ucts from natural materials. The solvating power of SC-CO2 fluids is
sensitive to temperature and pressure changes; thus, the extraction
parameters may be optimized to provide the highest possible extrac-
tion yields with maximum antioxidant activity for health-promoting
components in bioactive extraction production (Kassama et  al.,
2008; Yi et al., 2009).
A SC-CO2 fluid extraction process offers the unique advantage
of adding value to agricultural waste by extracting bioactives from
agricultural by-products, which are then used for the fortification
of foods and other applications. Its drawbacks are the difficulties
in extracting polar compounds and compounds from a complex
matrix, where the phase interaction with the intrinsic properties of
the product inhibits its effectiveness. These drawbacks can be ame-
liorated by using small amounts of food-grade co-solvents (less than
10%) to approach the high extraction efficiency (Shi et al., 2009).
The CO2 density, pressure, and temperature have been noted to have
great impacts on the results of the extraction process. When deter-
mining the parameters that should be used to maximize yields and
solubility of the targeted components, many researchers attempted
to use conditions that may be applicable in large-scale applications
(Shi et  al., 2007b; Kassama et  al., 2008). For example, non-toxic
co-solvents and modifiers could be acceptable for food processing;
therefore, a number of researchers have opted to use food-grade co-
solvents and modifiers in extraction processes (Shi et al., 2009). The
nature of the material used as a source of high-value components,
such as health-promoting components, governs the availability of
73
the compounds for the extraction process. The presence of other
components such as lipids may impede the process or elevate costs
due to an elongated extraction time.
Although a high temperature in the extraction process generally
increases the solubility of components in supercritical CO2 fluids, the
conditions under which thermolabile-targeted compounds are nega-
tively affected should be considered (Shi et al., 2007a, 2007c). The
intensity and the length of heat processing affect the health-promot-
ing properties of bioactives. Therefore, ideally, the extraction time
and temperature should be minimized. Minimizing such conditions
also leads to a more economically viable process (Shi et al., 2007b;
Kassama et al., 2008). Excessively high flow rates may reduce the con-
tact time between the solute and the solvent and restrict the fluid flow
in the sample if it becomes compacted. The optimal flow rate appears
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to vary with the targeted molecule, relatively high flow rates having
a negative effect on some components. Raising the pressure increases
extraction yields. Sample matrix is an important parameter that influ-
ences the solubility and mass transfer process during SC-CO2 extrac-
tion. Properties such as particle shape and size distribution, porosity
and pore size distributions, surface area, and moisture content influ-
ence solubility and mass transfer. The presence of water (moisture
content) in the sample matrix during supercritical extraction also has
an effect on the extraction outcome. In order to improve the yield
and quality of the extracted high-value food components from raw
material, a pre-treatment of the raw material is an essential process
(Yang et al., 2008; Zheng et al., 2009; Nagendra et al., 2010). Cell
disruption is the most important pre-treatment, and this procedure
can be conducted by several processes such as mechanical, ultrasonic,
high electronic field pulse, and non-mechanical treatments. With
improved processing conditions and reduced cost, high-value compo-
nents extracted from natural materials by SC-CO2 extraction process
will become even more economical at high throughput.
Pressurized low-polarity water extraction
Pressurized low-polarity water extraction, also known as SWE, that
is extraction using hot water under pressure, has recently become
a popular green processing technology and emerges as a promising
extraction and fractionation technique for replacing the traditional
extraction methods. The pressurized low-polarity water extraction
is also used in sample preparation to extract organic contaminants
from foodstuff for food safety analysis and solids/sediments for envi-
ronmental monitoring purpose. The pressurized low-polarity water
extraction process is an environmentally friendly technique that can
provide higher extraction yields from solid plant materials (Luque-de-
Castro and Jimenez-Carmona, 1998). Pressurized low-polarity water
extraction is based on the use of water as an extractant in a dynamic
mode, and under pressure high enough to maintain the liquid state.
The pressurized low-polarity water extraction process can maintain
the water in the liquid (Haar et al., 1984; Hawthorne et al., 2000).
A  pressure of 5  MPa would be high enough to prevent the water
from vapourizing at temperatures from 100 to 250°C. Once pressure
is high enough to keep water in a liquid state, additional pressure is
not necessary as it has limited influence on the solvent characteristics
of water. Increasing the water temperature from 25 to 250°C causes
similar changes in dielectric constant, surface tension, and viscosity
(Kronholm et  al., 2007; Brunner, 2009). Pressurized low-polarity
water extraction can easily solubilize organic compounds such as
phytochemicals, which are normally insoluble in ambient water.
Pressurized low-polarity water extraction has the ability to selec-
tively extract different classes of compounds, depending on the tem-
perature used. The selectivity of SWE allows for manipulation of the
74
composition of the extracts by changing the operating parameters,
with the more polar ones extracted at lower temperatures and the
less polar compounds extracted at higher temperatures (Basile et al.,
1998; Ammann et al., 1999; Clifford et al., 1999; Miki et al., 1999;
Kubatova et  al., 2001; Soto-Ayala and Luque-de-Castro, 2001).
Mazza and Pronyk (2015) designed an apparatus for extraction and
recovery of antioxidant components from biomass feedstocks with
pressurized low-polarity water. Their apparatus is configured with
two or more reaction columns, each separately communicating with
sources of pressurized water, pressurized heated water, and pressur-
ized cooling water. Components are extracted from the biomass by
separately flooding the column with pressurized water, heating the
column and its contents to the point, where the water becomes pres-
surized low-polarity water, recovering the pressurized low-polarity
water comprising the extracted components, cooling the column
with pressurized low-polarity water, and removing the spent biomass
material from the column. They concluded that the antioxidants can
be efficiently extracted by using this system.
Process  system.  The instrumentation consists of a water reservoir
coupled to a high-pressure pump to introduce the pressurized low-
polarity water into the system, an oven, where the extraction cell is
placed and extraction takes place, and a restrictor or valve to maintain
the pressure (Kronholm et al., 2007). Extracts are collected in a vial
placed at the end of the extraction system. In addition, the system can
be equipped with a cooling system for rapid cooling of the resultant
extract. The unique properties of the pressurized low-polarity water
extraction are as follows: it has a disproportionately high boiling point
for its mass with a high dielectric constant and a high-polarity nature.
As the temperature rises, there is a marked and systematic decrease
in permittivity, an increase in the diffusion rate, and a decrease in the
viscosity and surface tension of the polar materials.
The high degree of association of polar material in the liquid
causes its relative permittivity (more commonly called its dielectric
constant) to be very high at ca. 80 under ambient conditions. But
as the temperature rises, the hydrogen bonding breaks down and
the dielectric constant falls. The most outstanding feature of this
leaching agent is the easy manipulation of its dielectric constant (ε).
In fact, this parameter can be changed within a wide range just by
changing the temperature under moderate pressure. Thus, at ambi-
ent temperature and pressure, water has a dielectric constant of ca.
80, making it an extremely polar solvent. This parameter is drasti-
cally lowered by raising the temperature under moderate pressure.
The subcritical water at 250°C with a pressure over 40 bar has
ε = 37, which is similar to ethanol, and therefore, it easily allows for
the leaching of low-polarity compounds and thus between 100 and
200°C, this superheated water, which behaves like a water–metha-
nol mixture, so that the efficient extraction of targeted compounds
occurs.
The solubility of an organic compound with an solvent possess
many orders of magnitude, which has even got low degree of solu-
bility, when compared to water at ambient temperature, this may be
because of two reasons: first is the polarity change and second, the
compound with low solubility at ambient temperature. Pressurized
low-polarity water will have a high positive enthalpy of solution and
thus a large increase in solubility with temperature. Because of the
greater solubility of some organic compounds in superheated water,
this medium can be considered for the extraction and other processes,
to replace conventional organic solvents. But some additional reac-
tions of the compounds being processed may also occur, by hydrolysis,
oxidation, etc.
M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1
Industrial applications. Using pressurized low-polarity water pro-
vides a number of advantages over traditional extraction techniques
(i.e. HD, organic solvents, SLE). These are mainly shorter extraction
times, higher quality of the extracts (mostly for essential oils), lower
costs of the extracting agent, and an environmentally compatible tech-
nique. Since water is perhaps the most environmentally friendly sol-
vent available in high purity and at low cost, it has been exploited for
the extraction of avoparcin in animal tissue (Curren and King, 2001),
fungicides in agricultural commodities (Pawlowski and Poole, 1998),
fragrances from cloves (Rovio et al., 1999), antioxidative components
from sage (Ollanketo et al., 2002), anthocyanins and total phenolics
from dried red grape skin (Ju and Howard, 2003), saponins from
cow cockle seed (Guçlu-Ustundag et  al., 2007), and other bioactive
components from plant materials (Ong and Len, 2003). Some addi-
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tional successful applications of this technique are for the extraction
of essential oils from various plant materials (Khajenoori et al., 2009;
Mortazavi et al., 2010), extraction of sweet components from Sirai-
tia grosvernorii, extraction of lactones from kava roots, extraction of
antioxidant compounds from microalgae Spirulina platensis (Ibanez
et al., 1999, 2003), extraction of Ginkgo biloba, and extraction of bio-
phenols from olive leaves (Japon-Lujana and Luque-de-Castro, 2006).
The quality of the oil obtained is therefore better than that from
steam distillation, as it contains more of the oxygenated compounds
and lower terpene content. The yield is also slightly higher than
from steam distillation, in spite of the fact that all the terpenes are
not extracted. This may be because, at the higher temperatures and
under pressure, the plant material is more effectively penetrated.
However, about twice the amount of water is required than for
steam distillation. Energy costs are much less than for steam distil-
lation. The energy required to heat a given mass of water from 30
to 150°C under pressure is one-fifth of that needed to boil water at
atmospheric pressure from 30°C.
Molecular distillation
Distillation is a unit operation mainly used for the separation of the
mixture constituents by means of partial evaporation. It is based
on the fact that the vapour is relatively richer in the component
with the highest vapour pressure, i.e. the more volatile component.
Distillation at moderate vacuum is characterized by the use of con-
ventional distillation equipment. It is lowest pressure limit is on the
order of 1 torr, i.e. 1 mm Hg. When the distance of transfer is compa-
rable with the mean free path of the vapour molecules, then the dis-
tillation is known as molecular distillation. Mean free path is defined
as the average distance a molecule will travel in the vapour phase
without colliding with another vapour molecule (Eckles et al., 1991).
This implies that, in the molecular distillation system, the vapour
molecules can reach the condenser without intermolecular collisions.
Therefore, a dynamic equilibrium cannot be established between the
vapour and the liquid phase (Eckles et al., 1991).
Molecular distillation occurs at very low temperatures, and
therefore, it reduces the problem of thermal decomposition. High
vacuum also eliminates oxidation that might occur in the presence
of air. In molecular distillation, the rate of evaporation is controlled
by the rate at which the molecules escape from the free surface of
the liquid and condense on the condenser. For this separation pro-
cess, it is necessary to reveal the behaviour of target components
in the evaporation process. A molecular distillation procedure was
developed to extract the tocotrienols and other minor components
from palm fatty acid distillates (PFAD) (Posada et  al., 2007). The
effects of feed flow rate and temperature of distillation on extraction
Recent advances in extraction of antioxidants, 2017, Vol. 1, No. 1 75

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Figure 8.  Illustration of (a) a thin-film evaporator (TFE) unit and (b) short-path evaporator (SE) unit (modified from Ketenoglu and Tekin, 2015).

of minor components from PFAD were studied in terms of concen-

trations, distribution coefficients, and relative volatilities. The minor
components were concentrated in the liquid phase at low tempera-
tures and in the vapour phase at high temperatures. The separation
of tocotrienols from FFA approached maximum values only at low
temperatures and fell drastically as temperature increased.
A study was conducted to determine the antioxidant activity of
fractions separated from oregano essential oil by short-path molecu-
lar distillation process (Olmedo et  al., 2014). Two residues (R1 and
R2) and two distillates (D1 and D2) fractions were prepared by this
process. The major components identified were as follows: carvacrol,
terpinen-4-ol, and γ-terpinene in R1 and R2 residues; γ-terpinene,
α-terpineol, and sabinene in D1 and D2 residues. Free radical scaveng-
ing activity was also observed in all fractions and results shows that, it
was highest in R2 residue (77.2%). It was further concluded that the
short-path molecular distillation fractions can be successfully used to
prepare fractions from oregano essential oil with a higher antioxidant
activity. Zhang et al. (2013) studied the effects of evaporation tempera-
ture, feeding rate, feeding temperature, and wiper speed on concentra-
tion of ω-3 fatty acids by molecular distillation process. Researchers
reported the optimum conditions as 110.4°C evaporator temperature,
78.7 ml/h feeding rate, 350 rpm wiper speed, 10 MPa operating pres-
sure, and 80°C feed temperature for concentration of ω-3 fatty acids.

Process  system.  In molecular distillation process, there are two

different types of evaporators were used, i.e. thin-film evaporators
(TFE) (Figure 8a) and short-path evaporators (SE) (Figure 8b). In
both evaporators, feed is agitated with a rotor wiper system and
high vacuum is produced by vacuum pumps. In TFE, ­operating
pressure can be reduced to 1–100 mbar (UIC GmbH, 2014), and
there is no other unit between vacuum and condenser (Pilodist,
2014). In SE, condenser is placed in the centre of evaporator unit;
therefore, the distance between boiling and condensation surface
is extremely reduced and pressure drop is also minimized. The
operating pressure can be reduced up to 0.001  mbar. Distilla-
tion performed by a SE, which is known as molecular distillation,
and its illustration are given in Figure 8a and 8b. (Pilodist, 2014;
Technoforce, 2014). Xu et al. (2002) described certain important
parameters for molecular distillation process, which includes
evaporator temperature, flow rate, vacuum, and wiper speed. They
explained that the flow rate, which has got most important desir-
able effect over the contact time of the molecules, when the mol-
ecule is exposed to hot surface during evaporation process. Higher
flow rates may reduce the residence times of molecules, which are
being vapourized, and wiper speed also affects the film thickness
Figure  9.  A typical industrial fractional vacuum distillation plant (modified
from Jiang et al., 2006).
and viscosity. The feed also becomes highly turbulent with inten-
sive agitation, which leads to high heat-transfer coefficients (Buss-
SMS-Canzler GmbH, 2014).
Molecular distillation applications.  Molecular distillation, charac-
teristics of low pressure and low temperature, has great potential
for the separation, purification, and concentration of natural prod-
ucts, with complex and thermally sensitive molecules. The advan-
tage of this process is that it can be operated at higher vacuum with
shorter time period. A commercial production of a typical industrial
fractional vacuum distillation plant is shown in Figure 9. The effects
of feed flow rate and distillation temperature on the extraction of
76 M. Selvamuthukumaran and J. Shi, 2017, Vol. 1, No. 1

Table 4.  Extraction conditions of conventional solvent extraction, UAE, MAE, and SC-CO2 methods. MAE, microwave-assisted extraction;
SC-CO2, supercritical carbon dioxide extraction; UAE, ultrasound-assisted extraction.

Extraction method Conditions of extraction Characteristics

Conventional solvent Ethanol (80%), m/v: 5 g: 50 ml, 30 min, 35°C, me- —

extraction chanical stirring at darkness, 3 successive extractions
UAE Ethanol (80%), m/v: 5 g: 50 ml, 30 min, 35°C, magnet- Ultrasound sonicator (VibraCell 75115,
ic stirring at darkness, 3 successive extractions, 125 W Bioblock-Fisher, Illkirch, France)
MAE Ethanol (80%), m/v: 5 g: 50 ml, 10 s, 35°C, 170 W, 3 Microwave oven (WAVEDOM LG,
successive extractions France)
SC-CO2 Ethanol (80%), m/v: 5 g: 50 ml, 30 min, 35°C, 22 MPa, Pilot-scale extractor (ENSIC, LRGP,
3 successive extractions Nancy, France)

Source: Hiri et al. (2016).

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minor components are related to the yield, purity, and rate of evapo-
ration in terms of concentrations processes, which have gained wide
applications for products such as those derived from refined veg-
etable oils, e.g. deodorizer distillate of vegetable oils, palm oil for
obtaining tocotrienols and tocopherols, rice oil for oryzanol recov-
ery, monoglyceride concentration, carotenoid recovery from palm
oil, heavy petroleum characterization, and herbicides (Barnicki
et al., 1996; Shi et al., 2007b). A new process of molecular distil-
lation was also developed for recovery of tocotrienols and toco-
pherols from rapeseed by a combination of acid-catalyzed methyl
esterification and crystallization followed by fractional distillation
of derived products and for the recovery of orange peel oil and
essence products rich in aldehydes, esters, and other special volatile
compounds (Lutisan et al., 2002; Jiang et al., 2006).
Summary
The comparative effect of conventional solvent extraction, UAE,
MAE, and SC-CO2 on the total phenols content, total flavonoids,
individual flavonoids, and antioxidant activity of orange peel was
studied (Hiri et al., 2016). The method that gives the highest total
phenol and flavonoid content is MAE, followed by UAE, conven-
tional solvent extraction, and SC-CO2 extraction. Orange peel
extracted by conventional solvent extraction (Table 4) results in the
higher radical scavenging capacity compared to the other extracts
obtained by MAE, UAE, and SC-CO2 extraction methods. MAE
was found to be a better approach than UAE, conventional solvent
extraction, and SC-CO2 extraction methods in terms of phenols,
flavonoids contents, and individual flavonoids. MAE showed many
advantages, such as shorter time, higher extraction rate, the sav-
ing of energy, and better products with lower cost compared to
SC-CO2, which need high investments on large scale. The results
demonstrated that MAE can substitute the traditional conventional
solvent extraction process, which is a time-consuming technique
for efficient extraction of orange peel phenolic compounds.
Effects of solvent type, solvent to solid ratio, particle size, tem-
perature, and time on the total phenol content, DPPH, FRAP, and
extraction yield in different methods of extraction of antioxidants
from pistachio hull were studied (Tabaraki and Ghadiri, 2016).
MAE method showed the best effect on the extraction of antioxi-
dants from pistachio hull. The shortest process time was observed
for MAE (150-s irradiation time, total time of 21 min) with respect
to UAE (45  min) and conventional methods (90  min). The energy
consumption was 300 W × 2.5 min and 140 W and 45 min for MAE
and UAE, respectively. Thus, MAE method gave better results than
UAE and conventional methods with the optimum operating condi-
tions such as time and energy consumption. Other methods such as
PLE and SFE were also being used in the extraction of plant mate-
rials. These methods are less popular due to high cost despite the
efficiency of the methods (Azwanida, 2015).
The ever-growing demand to extract plant bioactive compounds
encourages continuous search for convenient extraction methods.
Replacing conventional technologies by non-conventional ones for
the extraction of valuable compounds from plant by-products pro-
cessing industries represents numerous advantages including the
reduction of the consumed energy, non-toxic organic solvents, and
the increase of the extraction yields, in full correspondence with
green extraction concept. Furthermore, some non-conventional
technologies are able to extract selectively the intracellular mole-
cules without fragmenting the treated tissue, which is highly sought
to reduce the subsequent purification steps. Incorporation and
development of hybrid methods should also be investigated con-
sidering plant material characteristics and choice of compounds.
The increasing economic significance of bioactive compounds and
commodities rich in these bioactive compounds may lead to find
out more sophisticated extraction methods in future.
Conflict of interest statement. None declared.
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