Green Extraction Methods for Polyphenols from

Plant Matrices and Their Byproducts: A Review

Kashif Ameer, Hafiz Muhammad Shahbaz, and Joong-Ho Kwon

Abstract: Polyphenols as phytochemicals have gained significant importance owing to several associated health benefits
with regard to lifestyle diseases and oxidative stress. To date, the development of a single standard method for efficient
and rapid extraction of polyphenols from plant matrices has remained a challenge due to the inherent limitations of
various conventional extraction methods. The exploitation of polyphenols as bioactive compounds at various commercial
levels has motivated scientists to explore more eco-friendly, efficient, and cost-effective extraction techniques, based on
a green extraction approach. The current review aims to provide updated technical information about extraction mech-
anisms, their advantages and disadvantages, and factors affecting efficiencies, and also presents a comparative overview
of applications of the following modern green extraction techniques—supercritical fluid extraction, ultrasound-assisted
extraction, microwave-assisted extraction, pressurized liquid extraction, and pressurized hot water extraction—as alter-
natives to conventional extraction methods for polyphenol extraction. These techniques are proving to be promising for
the extraction of thermolabile phenolic compounds due to their advantages over conventional, time-consuming, and
laborious extraction techniques, such as reduced solvent use and time and energy consumption and higher recovery rates
with lower operational costs. The growing interest in plant-derived polyphenols prompts continual search for green and
economically feasible modern extraction techniques. Modern green extraction techniques represent promising approaches
by virtue of overcoming current limitations to the exploitation of polyphenols as bioactive compounds to explore their
wide-reaching applications on an industrial scale and in emerging global markets. Future research is needed in order to
remove the technical barriers to scale-up the processes for industrial needs by increasing our understanding and improving
the design of modern extraction operations.
Keywords: microwave-assisted extraction (MAE), polyphenols, pressurized liquid extraction (PLE), pressurized hot water
extraction (PHWE), supercritical fluid extraction (SFE), ultrasound-assisted extraction (UAE)

Introduction
Plant phenolic compounds have considerable significance as
bioactive compounds with substantial health benefits. There are
several key factors responsible for the shifting trend toward herbal
products among the consumer markets of polyphenols globally.
Prominent factors include the rising proportion of aged people in
the populations of Japan and Europe, increased health awareness
of consumers, and the onset of various metabolic disorders due to
aging (Cherniack 2011; Visioli and others 2011).
A recent study conducted by Transparency Market Research,
a global market intelligence group, has predicted a boom in the
polyphenol market owing to increasing demands and market size.
This study indicates that the global demand for polyphenols in
2018 will be expected to reach USD 873.7 million. The estimated
demand is based on revenue (USD million) and volumes (tons)
CRF3-2016-1533 Submitted 9/20/2016, Accepted 12/6/2016. Authors Ameer
and Kwon are with School of Food Science & Biotechnology, Kyungpook Natl. Univ.,
Daegu 41566, South Korea. Author Shahbaz is with the Dept. of Biotechnology, Yon-
sei Univ., 50 Yonsei-ro, Seodaemun-gu, Seoul 03722, South Korea. Direct inquiries to
author Joong-Ho Kwon (E-mail: jhkwon@knu.ac.kr, knujhkwon@hanmail.net).
for the period 2012 to 2018, with an annual growth rate of 6.1%
(Transparency Market Research 2016).
Implementation strategy for green extraction techniques
The implementation process of green extraction on an indus-
trial scale consists of 3 tiers related to the optimization of process
variables: raw materials, energy, and solvent consumption. The
3-tier implementation process is comprised of the following level-
based innovation and modification of existing protocols and tech-
nologies: (i) bringing about improvement by innovative designing
and ensuring compliance with optimization strategies (Chemat
and others 2012; Buckley and others 2013), (ii) exploitation of
inherently undedicated equipment, and (iii) exploration of new
alternatives to conventional solvents during the design of inno-
vative processes (Cravotto and others 2011; Mustafa and Turner
2011).
The current review aims to provide updated technical informa-
tion about extraction mechanisms, their advantages and disadvan-
tages, and also presents a comparative overview of the applications
of modern green extraction techniques—supercritical fluid ex-
traction (SFE), ultrasound-assisted extraction (UAE), microwave-
assisted extraction (MAE), pressurized liquid extraction (PLE), and


C 2017 Institute of Food Technologists®

doi: 10.1111/1541-4337.12253 Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 1
Polyphenols extraction by green methods . . .

pressurized hot water extraction (PHWE)—as alternatives to con- the CO2 -extract separator, the solvation power of the SC fluid is
ventional extraction methods (for example, Soxhlet, percolation, lowered by combined manipulation of temperature/pressure. The
and maceration). phenolic compounds dissolved in the fluid are separated from the
fluid in the CO2 -extract separator by means of an outlet valve
Extraction techniques for plant-derived polyphenols located on the lower side of the separator. The cyclic process of
Plant materials have been increasingly exploited to isolate and SFE continues until maximum recovery rates of polyphenols are
purify bioactive compounds, and recent studies have reported on achieved from the targeted plant sample matrices (Wang and Weller
the antioxidant potential of byproducts of fruits (Shahbaz and 2006).
others 2016a, 2016b). Traditional techniques involve application
of solid–liquid extraction (SLE) simply by means of solvent ap- Factors Influencing SFE Efficiency
plication and leaching. A domestic application of conventional Correct SC fluid selection
solvent extraction (CSE) is quite familiar to everybody in daily This is one of the crucial factors governing SFE efficiency for
life from the making of coffee or tea at home. SLE encompasses polyphenol extraction. Due to the thermolabile nature of pheno-
conventional methods: Soxhlet extraction (SE), percolation, and lic compounds, SC water is not a good choice in spite of high
maceration extraction (ME). These techniques have been utilized extraction yields in the case of polar compounds. Polyphenols
for more than a century for the isolation of polyphenols. However, possess a low degree of solubility in SC-CO2 , making CO2 usage
certain disadvantages pertaining to CSE render its application quite alone unfavorable (King 2014). To overcome this limitation, mod-
uneconomical due to excessive consumption of time, energy, and ifiers have been added to SC-CO2 in order to improve solubility
polluting solvents (Cravotto and others 2011). These underlying and recovery rates of phenolic compounds. Acetonitrile, acetone,
drawbacks have triggered research that explores more cost-effective methanol, ethyl ether, ethanol, and water are the most commonly
and greener techniques for the extraction of polyphenols from a used effective polar modifiers (Pereira and Meireles 2009; Azmir
wide range of plant matrices and their byproducts (Azmir and and others 2013). Ethanol has been reported to be the better op-
others 2013), as illustrated in detail in Figure 1. tion as a modifier compared to others by virtue of its lower toxicity
and enhanced extraction of polyphenols with a lower degree of se-
SFE lectivity. Water has very low solubility in SC-CO2 and is normally
In a broad sense, SFE has established itself as a prominent green not used as a modifier alone. In order to increase water solubility,
method, particularly in the case of solid matrices, owing to the binary mixtures of ethanol and water are used (Wang and Weller
advantages described in Table 1. SFE has been widely used for 2006; King 2014).
value-addition to plant byproducts generated during processing.
Such products apparently have no commercial significance, and Modifier effect
extraction allows effective exploitation of waste components in Clean extracts with higher recovery rates are achieved by ex-
order to extract the targeted phenolic compounds (Herrero and ploiting a temperature range just above the critical point at which
others 2010). the targeted phenolic compounds have solubility in a fluid. This
also helps to minimize the extraction of unwanted compounds
Extraction principle and mechanism of SFE from matrices. Modifiers can also influence extraction efficiency
Supercritical (SC) fluid can be defined as fluid existing in a during the SFE operation (Wang and Weller 2006). Higher extrac-
phase which possesses features of both liquids and gases above its tion rates of a glycosylated flavonoid (naringin) have been reported
characteristic critical temperature and pressure. Critical pressure from Citrus paradise when ethanol (15%) was used as modifier with
(Pc ) is regarded as the minimum quantity of pressure required to SC-CO2 at 331.83 K (Tc ) and 5.9 to 9.5 MPa (Pc ), as compared
liquefy a gas at its unique critical temperature. The critical tem- to the yield obtained using SC-CO2 alone. SFE results in a higher
perature (Tc ) of a gas is the temperature at which the gas does not yield (14.4 g/kg in 45 min) in comparison with the yield rates
become liquid until application of extra pressure. SC fluids have obtained from ME (11.1 g/kg in 24 h) and heat reflux extraction
become solvents of choice due to the combined properties of 2 (HRE) (13.5 g/kg in 3 h) (Giannuzzo and others 2003).
individual phases: gaseous and liquid simultaneously. This results
in an improved mass transfer rate of solutes during extraction. Particle size effect
Hence, SC fluid provides unique properties of viscosity, density, Particle size is another factor that has an influential effect on SFE
and solvation at a phase between liquids and gases. These proper- efficiency during phenolic compound extraction. Particle size is
ties can be modified by varying temperature/pressure (Lang and reported to influence mass transfer of solutes during the extraction
Wai 2001; Pereira and Meireles 2009). The SFE system is depicted process, thereby affecting polyphenol recovery rates (Pereira and
in detail in Figure 2. During the extraction process, plant raw Meireles 2009). In another study, the effect of particle size on SFE
material is fed into an extraction vessel. The desired extraction efficiency was investigated for the extraction of isoflavones from
conditions are maintained by the operation of a pressure release soybean meal. It was concluded that an optimum particle size in
valve and temperature controllers attached to the extraction vessel. the range of 20 to 30 mesh provides a greater surface area and, con-
European Food Safety Authority and the United States Food and sequently, results in increased mass transfer. Improved isoflavone
Drug Administration have assigned CO2 a generally recognized yield was obtained because of enhanced extractant penetration in
as safe (GRAS) status. CO2 is the most widely used SC solvent the matrix. Any deviation of particle size—less than 20 mesh or
because of its particular features, notably its economic inexpen- greater than 30 mesh—leads to a marked decline in isoflavone
siveness and GRAS status (Pereira and Meireles 2009; Herrero recovery from soybean meal (Zuo and others 2008).
and others 2010; Khosravi-Darani 2010). CO2 is pumped as a
fluid at critical conditions (Tc < 278.15 K and Pc = 5.7 MPa) to SFE applications for the green extraction of polyphenols
the extraction vessel. Heat exchangers are used to cool the CO2 Recently published studies have reported on the extensive ap-
located in the inlet and outlet of the CO2 pump (Figure 2). In plication of SFE in the food sector, due to the distinctive merits

2 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017 
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Polyphenols extraction by green methods . . .
Figure 1–Conventional and modern extraction methods for plant-derived polyphenols.
Figure 2–Operational schematic mechanism of supercritical fluid extraction (SFE) system.
of SFE. Promising features include its potential as a sustainable
and environmentally friendly technique that limits the use of toxic
organic pollutants, improved selectivity for isolating targeted com-
pounds, faster extraction rate, comparable yields, and utilization
of food-grade organic modifiers (Pereira and Meireles 2009; De
Melo and others 2014). Zuo and others (2008) extracted the soy-
bean isoflavones (predominantly daidzein, genistein, and daidzin)
from soybean meal, and the effects of various factors, such as mod-
ifier (aqueous methanol) concentration and operating conditions
(Pc , Tc , and SC-CO2 flow rate), were investigated. CSE was com-
pared with SFE in terms of isoflavone recoveries. After studying
the effect of various factors, a maximum isoflavone yield of 87.3%
was obtained with the following conditions: 80% aqueous modi-
fier, 50 MPa (Pc ) at 313.15 K (Tc ), 20 to 30 mesh as the optimum
particle size range, with SC-CO2 flow rate of 9.80 kg/h. SFE
of isoflavones was reported to be more efficient, with a 10.2%
increase in yield and rapid extraction time (the optimum is only
150 min), in comparison with CSE, which takes up to 4 h at
333.15 K, and may lead to degradation of thermolabile soybean-
meal isoflavones (Zuo and others 2008).

C 2017 Institute of Food Technologists®
Cajaninstilbene acid (CSA) and pinostrobin (PI) are, respec-
tively, a stilbene and flavonone from pigeon pea leaves and Kong
and others (2009) compared the antioxidant activities of SFE ex-
tracts of these compounds with those recovered by HRE. Af-
ter optimizing the SFE process by employing response surface
methodology (RSM), a statistical process optimization technique,
SFE resulted in enhanced recovery of CSA and PI under the fol-
lowing operating conditions: a Pc of 30 MPa with ethanol (80%)
as a modifier and a solid/liquid ratio of 10:1, a CO2 flow rate of
12 kg/h at Tc of 333.15 K, and extraction time of 2 h. Higher
yield rates of CSA (11.17 mg/g) and PI (2.73 mg/g) were achieved
in the case of SFE extracts with relatively higher antioxidant ca-
pacities compared to the HRE yield rates (8.31 and 1.99 mg/g
for CSA and PI, respectively). A higher SFE extract yield was
achieved due to an increased mass transfer rate. Table 3 shows a
comparative overview of SFE for polyphenols in comparison with
other green methods.
SFE process was optimized by RSM for effective and effi-
cient extraction of flavonoids from kudzu (Pueraria lobata) owhi
plant roots. The highest flavonoid contents were obtained at the
Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 3
Polyphenols extraction by green methods . . .

Table 1–Advantages, disadvantages, precautions, and applications of1 SFE,2 UAE,3 PLE, and 4 PHWE.

Sr. no. Merits Demerits Precautions Applications References

SFE
1) Cutting down usage of Extended time due to Provision of adequate Recovery of natural (Herrero and others
organic solvents low rate of diffusion contact time for products and 2010; Sairam and
and potential risk of of solute from solid proper solvent thermosensitive others 2012)
storage matrix in to the SCF penetration into polyphenols from
plant matrices for wide range of plant
diffusion matrices
2) Reduction in Imprecise modeling Achievement of Phenolic compounds (Herrero and others
extraction time to can affect efficiency equilibrium (phase and flavors 2010; King 2014)
allow process of SFE equilibrium of r
completion in solvent and solutes) Ginger
r Eucalyptus
about 20 min due r
to back-diffusion of Soybean
r Coffee
analytes of interest r
in SFE process Orange peel

3) Possesses excellent Scalability is Byproducts recovery (Herrero and others

suitability for impossible due to from fruits and 2010; Sairam and
extraction of lack of molecular vegetables others 2012)
solid/liquid model of solutes
compounds with diffusion in to SCF
lower volatility
4) Requirements of Requirements for high (Ghude and others
operative pressures of SC 2013; King 2014)
conditions are fluids and costly
relatively lower infrastructure such
as CO2 pumps and
pressure vessels
5) Allows maximum Variation may be (Sairam and others
degree of brought about in 2012; King 2014)
separation of terms of
solvent from target consistency and
extract reproducibility of
continuous process
of extraction
6) Continual process with CO2 cannot always be (Herrero and others
no intermittence used as SC solvent 2010; King 2014)
due to its nonpolar
nature for polar
solutes
7) Cost-effective Postextraction (Herrero and others
handling residual solvents 2010; Sairam and
disposal issues from others 2012)
plant matrices
complying to EPA
regulations
8) Ease in recovery of (Sairam and others
employed solvent 2012; King 2014)
9) Usage of cosolvents (Sairam and others
with cosolutes 2012; King 2014)
result in enhanced
efficiency
UAE
1) Ease of use due to Availability of solvent Careful Extraction and (Vilkhu and others
simplicity of is necessary in order experimentation recovery of natural 2008; Tadeo and
technique to carry out required to choose products others 2010)
optimum extraction optimum solvents
of bioactive for high recovery
compounds
2) Increased extraction Degradation of active Nondestructive (Vilkhu and others
throughput of principles from method for 2008; Kentish and
extracted materials plant matrices extraction of active Feng 2014)
and rapid occurs due to principles from
extraction rate of oxidative pyrolysis vegetable matrices
thermolabile caused by hydroxyl
components at (OH-) radicals
mild/low during cavitation
temperature ranges phenomenon
during processing
3) Increased extraction Degradation of active Nondestructive (Vilkhu and others
throughput of principles from method for 2008; Kentish and
extracted materials plant matrices extraction of active Feng 2014)
and rapid occurs due to principles from
extraction rate of oxidative pyrolysis vegetable matrices
thermolabile caused by hydroxyl
components at (OH-) radicals
mild/low during cavitation
temperature ranges phenomenon
during processing
(Continued)

4 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017 
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Polyphenols extraction by green methods . . .

Table 1–Continued

Sr. no. Merits Demerits Precautions Applications References

4) Less time consuming High ultrasound Extraction of (Vilkhu and others
as compared to waves bring about polyphenols from 2008; Kentish and
traditional deleterious effects plant matrices/ Feng 2014)
techniques, such as, in active byproducts or waste
Soxhlet extraction, constituents in parts (bark, leaves,
maceration and plants by free peel, and seeds)
hydrosilization) radical formation
and result in
undesirable
changes in
extracted
components
5) Low cost and Dilution of extract is Intensification of (Knorr and others
economically viable one of the major bioactive 2011; Simsek and
choice for green drawbacks in case compounds others 2012)
extraction of of dynamic (polyphenols) from
polyphenols ultrasound-assisted natural plant
extraction (DUAE) sources
6) Advantageous due to (Tadeo and others
diminishing 2010; Awad and
laboratory wastes others 2012)
7) Coupling with other (Tadeo and others
techniques such as, 2010; Kentish and
MSPD, enables Feng 2014)
enhanced
extraction of plant
matrices without
further purification
8) Maximum (Kentish and Feng
compatibility of 2014)
UAE with GRAS
solutions
9) Ultrasounds allow (Vilkhu and others
penetration of 2008; Awad and
solvents to greater others 2012)
depths in sample
matrices to
facilitate the
increased mass
transfer of solutes
to extraction
solvent
10) Minimum degree of (Awad and others
interaction of 2012; Kentish and
ultrasonic waves Feng 2014)
with extracted
materials during
extraction process
PLE
1) Extraction of target Requirement of Care must be taken to Polyphenols and (Mustafa and Turner
analytes efficiently sophisticated and select solvent nutraceuticals from 2011; Knorr and
in faster manner specialized mixtures from wide wide range of plant others 2011; Heng
from solid plant automated range of choices, matrices and others 2013)
matrices equipment especially modifier
and surfactant
assisted in terms of
sustainability and
safety
2) Increased wetting of Economic Bioactive compounds (Mustafa and Turner
matrix molecules by consideration due from herbal sources 2011; Knorr and
solvent and requirement of r Isoflavones others 2011; Heng
enhanced various columns r Flavonones and others 2013)
penetration (Silica gel) for r Antioxidants
removal of food
samples in
destructive manner
3) Reduced viscosity of Need for continual (Carabias-Martı́nez
employed solvent improvement of and others 2005;
at elevated automation levels Knorr and others
temperature and for reduction of 2011)
pressures, resulting sample preparation
in increased bottlenecks with
solubility analyst
intervention to
minimum degree
(Continued)


C 2017 Institute of Food Technologists® Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 5
Polyphenols extraction by green methods . . .

Table 1–Continued

Sr. no. Merits Demerits Precautions Applications References

4) Increased mass Lower recovery rates (Carabias-Martı́nez
transfer by of potentially and others 2005;
facilitating thermosensitive Mustafa and Turner
breakdown of polyphenols at 2011)
matrix-analyte elevated
bonds facilitating temperatures
solute diffusion
from plant matrix
5) Reduced time and Incomplete extraction (Mustafa and Turner
solvent usage with under static mode 2011; Santos and
advantage of online due to limited others 2012)
coupling with extractant volume
instrumental
separation
techniques (GC &
HPLC), and
automation
PHWE
1) Employment of water Addition of different Maintenance of Extraction of (Teo and others 2010;
as eco-friendly additives and constant pressure numerous phenolic Plaza and Turner
extractant with purpose-based to ensure subcritical compounds 2015)
similar polarity to modifiers may water conditions (Flavonoids and
that of organic result in alteration nonflavonoids) from
solvents (for of physicochemical vast range of plant
example, alcohol) properties of matrices
with minimum superheated water
disposal issues r Anthocyanins
2) Facilitates diffusion of Requirement of r Hydroxycinnamic (Teo and others 2010;
variety of solutes micelle-mediated Vergara-Salinas
within range of low PHWE with Triton acids and others 2015;
r Flavonols
to medium X-100 for r Plaza and Turner
polarities with thermosensitive Flavones 2015)
r Flavonols
improved selectivity components r Flavanols
r p-coumaric acid

3) Reduction of organic (Vergara-Salinas and

solvents usage to others 2015)
greater extent
4) Nontoxic and (Teo and others 2010;
cost-effective Plaza and Turner
extraction 2015)
technique of
organic
components from
wide array of plant
matrices/
byproducts
5) Low operational and (Vergara-Salinas and
maintenance others 2015)
requirements as
compared to other
sophisticated
techniques
6) Improved aid in (Vergara-Salinas and
bioremediation others 2015)
procedures as being
green extraction
method
1 SFE (Supercritical fluid extraction).
2 UAE (Ultrasound-assisted Extraction).
3 PLE (Pressurized fluid extraction).
4 PHWE (Pressurized hot water extraction).

following set conditions: a Tc of 323.15 K, SC-CO2 flow
rate of 20 L/h, with approximately 181 mL ethanol modi-
fier at a Pc of 20 MPa (Wang and others 2008a). Ethanol
used as cosolvent caused an increased polarity of SC-CO2,
which resulted in improved extraction yields of flavonoids
from plant roots. Moreover, the model-predicted values showed
a fair match with experimental values under optimum
conditions.
Rice wine lees was investigated for antioxidant activity of phe-
nolic compounds from SFE extracts. Ethanol (as the employed
modifier) in combination with SC-CO2 has been described as a
critical factor for enhanced SFE efficiency for polyphenols. SFE
has been compared with SE in terms of extract yield and extrac-
tion times. SFE yielded 43% of total SE extract yield. In contrast,
the SFE process has been reported to consume considerably less
ethanol (approximately one-tenth of the amount used in SE) and
time (only 1 h compared to 6 h in the case of SE). Polyphenol
extraction was found to increase with a corresponding increase in
95% ethanol volume during SFE. A final yield rate of 11.9% was
reported using the following extraction conditions: Pc (35 MPa)
and Tc (313 K) with SC-CO2 flow rate of 25 mL/min (Wu and
others 2009).

6 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017 
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Polyphenols extraction by green methods . . .
UAE
UAE has emerged as a promising technique that fulfills the re-
quired criteria as an inexpensive green extraction technique. No-
table UAE features include versatility, simplicity, safety, rapidity,
eco-friendliness, and cost-effectiveness, due to the reduced con-
sumption of time, energy, and expensive organic solvents, which is
in contrast to traditional extraction techniques (Wang and Weller
2006; Azmir and others 2013). The advantages, disadvantages, and
limitations of UAE are presented in Table 1.
Extraction principle and mechanism of UAE
Acoustic waves are classified as longitudinal waves that require a
certain medium for their propagation. However, ultrasound waves
differ from normal sound waves by virtue of their relatively higher
frequencies than those of the normal audible range of humans
(ࣙ20 Hz to 20 kHz) (Priego-Capote and de Castro 2004; Azmir
and others 2013). As ultrasound has longer wavelengths, typically
in the millimeter (mm) range, which are longer than medium-sized
molecules, chemical changes are not brought about by the direct
interaction of waves with matrix molecules. Instead, chemical
changes are brought about due to phenomenal changes, resulting
in implosion caused by massive energy production (de Castro and
Delgado-Povedano 2014; Kentish and Feng 2014). Generally, the
most widely used extractor device for sonication is an ultrasonic
bath, as shown in Figure 3.
In order to conduct sonication for extraction purposes, the op-
erational frequencies of ultrasound waves generally range from 20
kHz or above. When media are exposed to such high frequencies,
ultrasound waves produce their effects by transmittance of massive
energy and pressure, which are radiated by base transducers to the
targeted sample causing cavitation (Figure 3). Strong ultrasonic
waves result in the formation of bubbles in liquid media upon
interaction with a matrix. The bubbles continue to absorb energy
up to their maximum limit, and further exposure to ultrasonic
waves causes the bubbles to grow and collapse; in sonochemistry,
this collapse is described as cavitation (Azmir and others 2013). As
a consequence of this collapse, a considerable amount of energy is
produced, which occurs in an uncontrollable manner in each di-
rection in the ultrasonic bath tank (Figure 3). This massive energy
release causes significantly extreme changes in temperature (up to
5000 K) and pressure (100 MPa) within bubbles during extrac-
tion, causing liquid solutes to leach at speeds of 280 m/s (Vilkhu
and others 2008; Vázquez and others 2014). Figure 3 provides a
detailed schematic overview of the UAE mechanism. Upon son-
ication, ultrasonic waves break up solid particles (disruption) and
remove inert material layers, which may cause passivation, result-
ing in an increased surface area for mass transfer of solutes during
extraction (Figure 3).
Factors Influencing UAE Efficiency
Operational conditions
Application of ultrasound during extraction influences other
process variables, namely, the extraction temperature and pressure.
A reduction in temperature occurs due to the applied ultrasound
during operation, making UAE a preferred choice for the extrac-
tion of thermosensitive phenolic compounds from a wide range of
plant matrices. However, it is noted that this temperature change
can be unfavorable in terms of extract recovery, due to changes
in extraction time. Consequently, temperature should be regulated
carefully during optimization studies (Wang and Weller 2006). Ma
and others (2008) have observed a declining trend in hesperidin

C 2017 Institute of Food Technologists® Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 7
yield from citrus peel due to thermal degradation of phenolic com-
pounds at elevated temperatures during longer extraction times.
Sonication parameters (power, temperature, and frequency).
Lower frequency has been reported to be correlated with in-
creased cavitation during UAE. Increased efficiency is obtained
due to the positive influence on mass transfer of solutes from plant
matrices. The porous nature of plant matrices is also found to be
affected by the applied frequency during sonication. This necessi-
tates optimization studies for enhanced extract yields of phenolic
compounds (Wang and Weller 2006). Hesperidin extract yield was
found to be higher (1077.62 mg/g DW) from Satsuma mandarin
peel under an optimum frequency of 60 kHz instead of 100 kHz,
303.15 K temperature for 20 min extraction time, and 8 W power,
compared to ME for 8 h, which resulted in a lower recovery rate
(601.2 mg/g DW). It was also noted that decreased recovery of
hesperidin was obtained with a gradual increase in extraction pro-
cess variables. Therefore, the authors stressed the need for carefully
optimized application of UAE (Ma and others 2008).
UAE applications for the green extraction of polyphenols. UAE
of isoflavones from Pueraria lobata (Wild.) ohwi stem was car-
ried out and extraction efficiency was compared with that of
CSE using aqueous solutions of n-butanol (95%) and ethanol of
2 concentrations: 95% (v/v) and 50% (v/v) (Huaneng and others
2007). The authors found UAE to be more efficient for total ex-
tract yield of isoflavones than CSE under the following extraction
conditions: 50% aqueous ethanol (extractant), 650 W ultrasonic
power at 298.15 K with agitation at 300 rpm. A positive cor-
relation was also observed between extract yield and ultrasonic
power. Similarly, UAE was used to carry out the extraction of
phenolic acids (caffeic acid, p-coumaric acid, ferulic acid, sinapic
acid, protocatechuic acid, and 4-hydroxybenzoic acid) from Sat-
suma mandarin (Citrus unshiu Marc.) peels and compared with
ME as a control. The authors investigated the effects of different
operational parameters on phenolic compound extraction from
peel matrix: sonication time (10 to 60 min), temperature levels
(288.15, 303.15, and 313.15 K) at different ultrasonic power lev-
els (3.2, 8, 30, and 56 W). Ultrasonic power resulted in higher
extract yields of phenolic acids than those obtained by conven-
tional ME for 8 h expressed in µg/g DW units as follows: caffeic
acid (UAE = 64.28, ME = 31.7), p-coumaric acid (UAE = 140,
ME = 63.1), ferulic acid (UAE = 1513, ME = 763), sinapic acid
(UAE = 133, ME = 132), protocatechuic acid (UAE = 15.8,
ME = 20.6), and 4-hydroxybenzoic acid (UAE = 34.1, ME =
23.5). However, degradation of phenolic acids was reported to
take place at high temperatures for longer periods of time under
UAE. Therefore, the UAE technique must be used carefully by
optimizing all parameters for extraction in order to avoid thermal
degradation of phenolic compounds. Maximum yields of pheno-
lic acids were reported using the following optimized operational
parameters: 20 min of extraction time at 303.15 K temperature
and 8 W ultrasonic power (Ma and others 2008).
The potential of UAE was exploited for a comparative study
with traditional mix-stirring (TMS) regarding the efficiency of ex-
tracting isoflavones from freeze-dried soybeans. The extract yield
of soy isoflavones was found to be higher in the case of UAE
extracts. Optimal UAE parameters for enhanced soy isoflavone
extraction at 333.15 K comprise a sonication power of 200 W for
20 min at 24 kHz frequency. Under these optimized conditions,
sonication led to an enhanced extract yield of isoflavones (1180
µg/g DW) from soybeans compared with that obtained using the
TMS method (1098 µg/g DW), which was used as a control
(Rostagno and others 2003).
Polyphenols extraction by green methods . . .
Figure 3–Operational schematic principle of ultrasound-assisted extraction (UAE) system.
In another instance, UAE for anthocyanin, antioxidant, and to-
tal phenolic contents from grape seed was optimized by a central
composite rotatable design using RSM. Extraction time as a pro-
cess variable was reported to play an influential role in enhancing
the total extract yield of anthocyanins (2.29 mg/mL), total pheno-
lic content (5.41 mg GAE/mL), and increased antioxidant activity
(12.28 mg/mL). The optimal extraction conditions for antho-
cyanins were found to be an ethanol concentration of 53% and
326.15 K temperature for 29 min extraction time, while keeping
the ultrasonic power and frequency constant: 250 W and 40 kHz,
respectively. The authors reported a reasonable match between the
predicted and real values of response variables after optimization
(Ghafoor and others 2009).
In conclusion, UAE has a demonstrated edge over traditional
extraction techniques and has proven to be more suitable for
polyphenol recovery as a modern green extraction technique. Pe-
culiar features differentiating UAE from conventional techniques
include decreased solvent consumption, easy residual recovery
from plant matrix in bound form, rapid and substantial recov-
ery rates of polyphenols, and suitability of the UAE method for
routine analysis due to cost-effectiveness of equipment and in-
frastructure (Wang and Weller 2006; Vilkhu and others 2008).
Table 3 presents a comparative overview of the UAE of polyphenol
from various plant matrices in comparison with other extraction
methods.
MAE
Initially, all technologies collectively known as “microwave-
assisted processes (MAPs)” were developed and patented by the
Canadian Department of the Environment (Environmental Tech-
nology Centre). These methods were developed for the extraction
of bioactive compounds from various targeted plant matrices and
their byproducts. A review of the published literature indicates that
this technique is also acknowledged as a clean process technol-
ogy with several environmental, economic, and social advantages
(Kwon and others 2003a, 2003b). The advantages, disadvantages,
and limitations of MAE are tabulated in Table 1.
Principle and mechanism of MAE. MAE is an efficient and
promising method involving derivation of natural compounds
from raw plants or their byproducts. The MAE process allows
rapid and efficient extraction of polyphenols with similar or bet-
8 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017
ter yields as compared to conventional techniques (Abdel-Aal and
others 2014). Two oscillating perpendicular fields, electric and
magnetic fields, act directly to heat materials having the ability to
convert part of the absorbed energy to thermal energy. MAE of-
fers several advantages over CSE, including reduction in extraction
time, improved yield, better accuracy, and suitability for thermo-
labile chemical components (Delazar and others 2012; Azmir and
others 2013).
Dried plants contain minute microscopic traces of moisture
serving as target for microwave heating. High temperature and
pressure is generated inside the oven upon interaction of mi-
crowave radiation with chemically bound water molecules. High
temperature causes the dehydration of cellulose leading to de-
creased mechanical strength. The MAE process consists of several
steps in order to achieve efficient extraction of phytochemicals,
particularly polyphenols from plants (Veggi and others 2013). The
MAP starts with the generation of electromagnetic waves from a
cavity magnetron (Figure 4). Tissues and cell walls of plants and
their byproducts inside the plant matrix interact with the emit-
ted radiation waves. This interaction results in the heating up of
moisture trapped inside the plant matrix due to absorption of the
characteristic photonic energy of electromagnetic waves. Electro-
magnetic energy causes moisture evaporation from the plant ma-
trix. This causes considerable pressure to be exerted on plant cell
walls at the cellular and subcellular levels, resulting in the swelling
of plant cells during the MAE process. This swelling eventually
brings about structural changes in the plant matrix, thereby pro-
moting an increased mass transfer of solutes due to the rupturing
of cells. This, in turn, facilitates phytochemical leaching from the
plant cellular matrix into the extractant during MAE (Delazar and
others 2012; Azmir and others 2013; Veggi and others 2013).
Commercial MAE system types
Commercially, 2 types of MAE systems are available for indus-
trial and commercial applications for natural product extraction:
(i) the closed-vessel system and (ii) the open-vessel system (Figure
4). A comparison regarding the advantages and disadvantages of
commercial MAE systems for extraction purposes is presented in
Table 2.

C 2017 Institute of Food Technologists®
Polyphenols extraction by green methods . . .
Figure 4–Operational schematic principle and mechanism of microwave-assisted extraction (MAE) system. (a) Open-vessel MAE system. (b)
Closed-vessel MAE system.
Closed-vessel system (multimode)
In this system, extraction is carried out under controlled condi-
tions of temperature and pressure. This is generally employed for
extractions under extremely high temperature conditions (Wang
and Weller 2006). Diffused microwaves from a cavity magnetron
radiate in all directions to interact with plant samples placed in
extraction vessels in a closed-vessel chamber. Owing to the even
dispersion of microwaves, this technique is also known as the mul-
timode system (Figure 4).
Open-vessel system (monomode)
In this system, also known as the monomode system, the ex-
traction vessel is partially exposed to microwave radiation (focused
radiation) (Mandal and others 2007). A circular metallic waveguide
directs the focused microwaves toward the extraction vessel inside
the microwave (monomode) cavity. This interaction promotes the
initiation of mass transfer between the solute and extractant upon
solvation, as shown in Figure 4.
Factors Influencing MAE Efficiency
The efficiency of the MAE process is subjected to changes
caused by various factors: extractant nature, microwave irradiation
power, extraction temperature and time, the peculiar character-
istics of individual plant matrices, and the solvent-to-feed (S/F)
ratio. A detailed description of the factors influencing this tech-
nique is provided in the next section.
Microwave power
During the process of phenolic compound extraction, high mi-
crowave power levels can result in poor recovery rates due to
degradation of thermolabile components. It is noted that the ex-
traction rates of phenolic compounds from various plant matrices
have been shown to increase up to certain levels followed by a
declining trend in extraction yields. Evidently, the sample matrix
becomes heated because of localized interaction with microwaves.
This phenomenon leads to a higher diffusion of polyphenols out
of the plant matrix and into the extractant (Chan and others 2011).

C 2017 Institute of Food Technologists®
In the case of Oolong tea, the total phenolic content increased
with a rise in extraction temperature, and the optimum extract
yield was achieved at 443.15 K. Reduced yields were reported
beyond the optimum extraction temperature, confirming the im-
portance of an optimal combination of microwave power and
temperature for high extract yields of thermolabile phenolic com-
pounds from targeted plant matrices (Tsubaki and others 2010).
Extraction time. During MAE, the extraction time is an impor-
tant influential factor, along with microwave power and temper-
ature. As mentioned previously, exposure to microwave radiation
for longer time periods decreases overall extract yield due to dis-
ruption of the structural integrity of chemically active principles
(polyphenols) present in plant matrices. To circumvent thermal
degradation of phenolic compounds, extraction time during the
MAE process can be manipulated by controlling exposure, rang-
ing from a few minutes to 30 min, excluding the solvent-free
MAE. Moreover, in the case of longer extraction times, extrac-
tion cycles can be employed in order to reduce the degradation of
phenolic compounds. This can be accomplished by repetition of
the extraction procedure until completion, with subsequent ad-
dition of extractant during the extraction cycle (Chan and others
2011).
Pan and others (2003) have investigated the MAE process of
tea polyphenols and tea caffeine from tea leaves under vari-
ous experimental conditions. They found that MAE proved to
be more advantageous in terms of fast extraction with higher
yield rate. For the extraction of phenolic compounds from tea
leaves, MAE is completed in a shorter time interval (4 min) using
ethanol compared with CSE (20 h) at room temperature and HRE
(45 min).
Features of the plant matrix. Apart from other factors, the char-
acteristic nature and features of individual plant samples also in-
fluence efficiency of the MAE process. Prior to MAE, optimum
extraction of phenolic compounds demanded that the desired sam-
ple should be in particular forms: finely ground powdered sample,
dried, sieved, or preleached. Very small-sized sample particles will
Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 9
Polyphenols extraction by green methods . . .

Table 2–Comparison of closed-vessel and open-vessel MAE systems according to intrinsic advantages and disadvantages

Closed-vessel system Open-vessel system

Sr. no. Merits Demerits Merits Demerits References
1) Higher temperature, Application of high Enhanced and safer Comparatively exhibit (Zhang and others
constraints of pressure poses possibility of less precision than 2011; Veggi and
closed vessel system safety risks reagent addition in close-vessel others 2013;
renders reduced system Destandau and
extraction time others 2013)
2) Avoidance of loss of High solution Utilization of vessel Inability to process (Mandal and others
volatile substances temperature are manufactured from multiple samples 2007; Alupului and
not permissible by various materials simultaneously due others 2012;
constituent that is, quartz or to low throughput Afoakwah and Teye
material of vessel glass of equipment 2012)
3) Less solvent Impossibility of regent Easy removal of Longer time spans are (Zhang and others
requirement due to addition since it is excessive quantities required than 2011; Delazar and
absence of single step process of employed closed-vessel others 2012;
evaporation solvents system Alupului and others
phenomenon 2012)
4) No production of Constraint of cooling Easy processing of (Alupului and others
hazardous fumes down vessel before larger samples 2012; Afoakwah
during pressurized opening rendering volumes and Teye 2012)
extraction under prevention of
closed-vessel volatile
system constituents
5) High yield by using Handling and No need of (Zhang and others
ionic liquids (IL’s) at processing of operational cooling 2011; Afoakwah
ambient limited sample down or and Teye 2012;
temperature volumes depressurization Veggi and others
(70°F/294.26 K) 2013)
6) Simple procedural Requirement of Cost-effective (Delazar and others
set-up without any cooling step after availability of 2012; Veggi and
inherent complexity each treatment for sophisticated others 2013;
as compared to SFE further processing equipment for Destandau and
and other polyphenol others 2013)
techniques extraction
More effective for (Alupului and others
extraction of 2012)
thermosensitive
phenolic
compounds than
closed-vessel

lead to difficult separation of the extract from plant residues upon
completion of the extraction process. This will necessitate an ad-
ditional clean-up step after extraction of phenolic compounds
from plant matrices (Ruan and Li 2007; Chan and others 2014).
Furthermore, pretreatment of powdered samples with extractant
for 90 min prior to the extraction step has been reported to en-
hance MAE efficiency. This resulted in improved kinetics, such
as improved mass transfer and increased diffusion rate of phenolic
compounds from plant sample residues (Kaufmann and Christen
2002). In the case of dried plant sample matrices, pretreatment
with water has been reported to promote the heating effect of
microwaves in a localized manner. It was noted that heating up of
moisture present in the plant sample matrix continued to increase
as the extraction process progressed and resulted in higher evap-
oration rates. By allowing the release of polyphenols from plant
molecules due to matrix rupturing, this caused a further rise in
the internal pressure within the extraction cell, producing higher
extraction yields of phenolic compounds. A high moisture content
in plant matrices favors a high hydrolyzation tendency, which im-
proved the diffusion of solute molecules (Alfaro and others 2003;
Wang and Weller 2006; Mandal and others 2007; Azmir and others
2013).
Stirring effect. With the introduction of stirring during the
MAE process, the negative effects of the S/F ratio upon extraction
recovery can be minimized (Chan and others 2011). Furthermore,
concentrated polyphenols as bound active principles in the plant
matrix lead to the creation of a barrier to mass transfer rate due
to a deficiency of the extractant. Stirring action helps to reduce
this barrier, thereby enhancing the extraction yield by causing ac-
celerated agitation, which leads to increased extraction efficiency
(Ruan and Li 2007).
Effect of additives and solvent choice. Binary solutions of or-
ganic solvents with water were reported to have a desirable impact
on extraction efficiency. In this regard, it is also noted that the
presence of water in organic solvents leads to enhanced pene-
tration of the extractant in matrix molecules. This subsequently
promotes microwave heating and imparts a positive impact on
overall efficiency and extraction time compared with MAE using
organic solvents alone (Alfaro and others 2003; Wang and Weller
2006). Solvent toxicity is another important factor that must be
evaluated regarding the selection of a suitable extractant for MAE.
For instance, a recent study was conducted by Makris and others
(2015) to investigate the effects of solvent toxicity on the extrac-
tion of phenolic compounds from red grape pomace by utilizing 2
aqueous solutions of glycerol/tartaric acid. Upon optimization by
Box-Behken using the RSM approach, they concluded that glyc-
erol was a more suitable choice for enhanced flavonoid recovery.
Tartaric acid was found to exert a negative effect with regard to
phenolic compound recovery from grape pomace.
In the case of phenolic compound extraction from grape seeds
and skin, methanol has shown a relatively better performance
as an extractant in terms of higher recovery rates in contrast to
ethanol, which resulted in lower extract recovery with higher
antioxidant activity (Casazza and others 2010). MAE efficiency
was reported to be enhanced if the plant material is impregnated
with alternative solvents, such as an ionic liquid (IL) at room
temperature, in comparison with traditional organic solvents alone.
The advantages associated with IL addition include higher heating

10 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017 
C 2017 Institute of Food Technologists®
Polyphenols extraction by green methods . . .

efficiency, viscosity, tenability, and excellent thermal stability under PLE

microwave irradiation treatment (Mandal and others 2007). PLE is another green extraction technique for natural product
extraction from food and botanical sample matrices. The Dionex
MAE applications for the green extraction of polyphenols Corporation was the first to introduce the PLE technique as an
R
Colored grains from diverse origins (blue wheat, purple corn, ASE technology (ASE ) in 1995 (Benthin and others 1999). The
and black rice) are rich sources of polyphenols and the efficien- advantages, disadvantages, and limitations of PLE are presented in
cies of different methods used for their extraction have been Table 1.
compared: CSE, MAE, and accelerated solvent extraction (ASE)
for anthocyanins (water-soluble flavonoids). After optimization by Extraction principle and mechanism
full-factorial experimental design, higher extract recovery rates of Using PLE, a relatively faster extraction rate is attained due to a
anthocyanin from colored grains were achieved with both ASE combination of the following: (1) liquid solvent interaction with
and MAE compared to those obtained by CSE. ASE has been matrix molecules and (2) elevated temperature and pressure for
described as being more effective than MAE at the following op- efficient extraction of targeted components. Elevating the temper-
timum conditions: acidic methanol as solvent, 300 W power, and atures of employed solvents above their atmospheric boiling points
343.15 K temperature for 10 min. Anthocyanins were affected to allows increased solubility and mass transfer rates between the plant
minimal degree in terms of structural changes in the case of ASE matrix and the solvent of choice. Eventually, enhanced diffusivity
at the following set conditions: 100% flush by 5 cycles for 10 min of the solvent and plant matrix causes more prominent extraction
at 313.15 K and 17.24 MPa using aqueous acetone as a solvent kinetics. The application of elevated temperature decreases
(Abdel-Aal and others 2014). extractant viscosity, resulting in enhanced wetting of the plant
Dhobi and Hemalatha (2009) have compared MAE with con- matrix, and this leads to high solubility of the targeted molecules.
ventional methods, namely, ME (24 h), SE (12 h), and MSE It also causes breakage of bonding forces (dipole-dipole, van der
(24 h), for the extraction of silybinin (a flavonolignan) from the Waals, and H2 -bonding) in order to facilitate diffusion of targeted
roots of Silybum marianum. Owing to increased mass transfer, MAE phenolic compounds to the outer surfaces of solid matrices. Even-
has been reported to result in the highest extract yield (97.3%) as tually, increased diffusion rates allow high extraction efficiencies
compared to those obtained from MSE (35%), ME (26.3%), and with improved recovery rates (Carabias-Martı́nez and others 2005;
SE (79.6%). The optimum MAE conditions were reported to be Wang and Weller 2006). Figure 5 shows the basic set-up of a pres-
600 W of power, ethanol as solvent (80%), and an S/F ratio (25:1) surized liquid extractor. During the extraction process, the sample
at 12 min of extraction time. is placed into the extractor, followed by solvent pumping into the
MAE has been exploited for the extraction of health-promoting extraction vessel using an HPLC pump. The sample placed in the
flavonoids from artichoke herb (Cynara scolymus L.) leaves. The extraction cell is maintained at the desired temperature, using an
authors compared the efficiencies of MAE and CSE methods. electric heating jacket, until the required pressure is attained. After
The multimode MAE system was used for extraction purposes the desired combination of temperature and pressure variables is
under the following operational conditions; 313.15 to 523.15 K reached, the extraction process commences. Extraction processes
temperature, 0 to 400 W power, and 0 to 2 MPa pressure. MAE having more than 1 extraction cycles involve extraction solvent
efficiency was found to be better (74%) than CSE (70.5%) in terms replenishment during each extraction cycle. Owing to back
of flavonoid recovery yield under reduced extraction temperature pressure, blocking valves are opened carefully after completion of
(343.15 K) and time (1 to 2 min). The microwave power and pres- the extraction cycle at an appropriate level in order to maintain the
sure were described as temperature-dependent important process desired flow rate. Once the extraction process is completed, the
variables. The authors also highlighted the necessity for further heating system and HPLC pump are shut down. Inert gases such as
research to scale-up MAE as a green and rapid extraction tech- nitrogen may or may not be utilized for purging the pressurized
nique for thermosensitive phenolic compounds at an industrial liquid extractor for the removal of residual solvent within the
scale (Alupului and others 2012). Similarly, Routray and Orsat extractor.
(2014) identified high-bush blueberry (Vaccinium corymbosum) as
a potent source of flavonoids, particularly chlorogenic acids and Factors Influencing PLE Efficiency
anthocyanins. They evaluated MAE, UAE, and CSE techniques The factors that influence PLE extraction efficiency include
in terms of extraction efficiencies for flavonoids from the leaves matrix characteristics, choice of solvent, and extraction time and
of the Bluetta variety of blueberry. The authors reported on the temperature.
use of different levels of microwave power (10% to 20%) with Solvent choice and toxicity. When selecting a suitable extrac-
extraction times spanning from 4 to 16 min with 80 mL solvent tant, choice is always governed according to the famous notion
in combination with a 97:3 (v/v) ratio of 30% ethanol and 1.5 M “like dissolves like.” Therefore, an appropriate solvent and analyte
citric acid. Microwave power and extraction time were found to combination is necessary to achieve higher diffusion and mass
be positively correlated with a higher recovery yield of flavonoids. transfer rates, resulting in increased yield rates. Other factors that
MAE was claimed to be more efficient in terms of total phenolic must be taken into account in this regard include solvent safety and
content yield (92 to 128 mg GAE/g DW) compared to yields toxicity, along with economic aspects (Piñeiro and others 2004;
obtained by sonication for 1 h (97 mg GAE/g DW) and ordinary Plaza and others 2013). Non-harmful solvents with lower toxicity
room temperature extraction for 24 h (89 mg GAE/g DW) using and ease of removal are good choices. Solvents that are termed
the same combination of solvents. Therefore, MAE was reported as “green” should be preferred as they cause minimum environ-
to be the most efficient among all methods, followed by UAE, mental impact after their usage for extraction purposes. In PLE,
as an alternative method in circumstances where no MAE appa- various binary (mixture) solvents have been used for extracting
ratus is available. Table 3 presents a comparative overview of the phenolic compounds from various foodstuffs. Binary solvents
polyphenols extracted from various plant matrices using MAE as such as methanol-water or ethanol-water have been found to
a green extraction technique. be more effective and environment-friendly than pure organic


C 2017 Institute of Food Technologists® Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 11
 Table 3–Comparison of green extraction techniques for polyphenols from various plant matrices/plant byproducts.

Green extraction Plant Target phenolic Optimum extraction

Plant sample technique matrix/part compound parameters Extraction time Remarks Reference
Huáng qı́ (Radix MAE Dried root Flavonoids MP1 1000 W, 90% 25 min Higher yield rate than (Xiao and others 2008)
astragali) ethanol, extraction UAE and comparable
temperature (383.15 recovery with2 SE in
K), S/F ratio (1.190), 2 short time. In SE,
extraction cycles limited solvent choice
Chilean papaya UAE Seeds Isothiocyanates, 5 g papaya seeds+ 250 10 min UAE resulted in rapid and (Briones-Labarca and
phenolic acids, mL of 80% aqueous enhanced extraction of others 2015)
and flavanols methanol, 42 kHz F and phenolic compounds by
130 W UP3 of 4.23% as compared to4
ultrasound bath CSE techniques with
extractor reduced solvent and
energy
Sea-buckthorn MAE Fruit, leaves, and Flavonoids No solvent addition. 15 min 40% less yield of (Périno-Issartier and
seeds 400 W MP at power flavonoid (isorhamnetin others 2011)
density (1 W·g−1 ) 3-O-glucoside), higher
extract yield of
Polyphenols extraction by green methods . . .

reducing compounds as
compared to CSE
Citrus UAE Peel Flavonoids 60 kHz F at 313.15 K 60 min Excellent extraction (Londoño-Londoño and
temperature and efficiency than SE with others 2010)
methanol as solvent more choices of solvent
Red raspberry UAE Fruit Anthocyanins S/F ratio 4:1 (mL/g) and 200 s 78.13% recovery rate (Chen and others 2007)
400 W UP than 71.4% of CSE
Grapes UAE Fruit Flavonoids Water–ethanol (50:50), 6 min Higher recovery than (Carrera and others 2012)

12 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017
extraction temperature conventional reference
(273.15–348.15 K), UP method
and F, W and 24 kHz
Soybean MAE Beans Isoflavone 50% EtOH (25 mL), 500 20 min Similar recovery rate in (Rostagno and others
W MP at 323.15 K comparison with UAE 2007)
temperature but processing of 10
samples is possible
simultaneously with
MAE
Cortex fraxini MAE Bark Coumarins, 1.0 g sample in 40 mL 10 min 96% recovery rate of (Zhou and others 2011)
flavones polyethylene glycol extract yield, relatively
(PEG) solution, 338.15 higher than maceration
K temperature and reflux extraction
Hu Zhang Vacuum MAE and Leaves Resveratrol 95% methanol (40 mL), 15 min 6-9% increase in extract (Wang and others 2008b)
(Rhizoma MAE 328.15 K temperature, yield from VMAE than


Polygoni MP 600 W, vacuum MAE and 5 RE
Cuspidati) pressure (50 kPa) for
VMAE
Strawberry SFE Fruits Phenolic Modifier: Ethanol (0% to 60 min Rapid extraction of total (Akay and others 2011)
compounds 20%) with CO2. 60 min phenolics than CSE with
extraction time with a minimum solvent usage
flow rate of 15 g/min,
Tc (303.15 K) at 5 MPa
Pc
Orange UAE Peel Flavonoids Ethanol:Water ratio 4:1 30 min 35% to 40% increase in (Khan and others 2010)
(v/v) at 313.15 K and phenolic compounds
150 W UP than CSE
(Continued)

C 2017 Institute of Food Technologists®

 
Table 3–Continued.

Green extraction Plant Target phenolic Optimum extraction

Plant sample technique matrix/part compound parameters Extraction time Remarks Reference
Red bayberry VMAE Leaves Myricetin 50% ethanol (40 mL), 20 min Enhanced extraction of (Wang and others 2008b)
(Myrica rubra) at 333.15 K and 40 thermolabile phenolic
kPa, MP (600 W) compounds with better
recoveries in shorter
time periods than SE
Jabuticaba UAE Skin Anthocyanins Ethanol (99.5%) as 120 min Rapid and maximum (Santos and others 2012)
solvent, S/F ratio 10:1 recovery of
at 298.15 K anthocyanin than

C 2017 Institute of Food Technologists®

temperature and 81 W traditional LPSE
UP
Canola SFE Press cake/ meal Hydroxy-cinnamic 150 g canola press cake, 60 min Reduced extract recovery (Li and others 2010)
acid (Sinapine) modifier (95% ethanol) of phenolic compound.
with CO2 at Tc 323.15 Rapid and fast
K and Pc 400 MPa, with extraction in contrast
to CSE
Polyphenols extraction by green methods . . .

flow rate of CO2 at

70 g/min
Olive UAE Leaves Flavonoids 50% ethanol, 60 min Less consumption of time (Şahin and Şamli 2013)
sample/solvent ratio and solvent for
(500 mg dried leaf to comparable extract
10 mL), UP 220 W and yields with
F 50 kHz conventional reference
method
Apple MAE Pomace Flavonoids MP (650.4 W), ethanol as 53.7 s Higher recovery rates (Bai and others 2010)
solvent (62.1 mL) and than CSE, RE, and UAE
S/F ratio (22.9:1) techniques
Wine grapes SFE Seeds Flavonoids and 99.9% pure CO2 as 240 min SFE has provided efficient (Prado and others 2012)
phenolic acids solvent at Tc /Pc of recovery of phenolic
313 K/35 MPa to compounds than those
obtain SFE extracts at obtained by
S/F ratio of 6.6 conventional
distillation
Rosemary MAE Dried leaves Phenolic acids and 5 g of sample in methanol 5 min Comparable recoveries of (Švarc-Gajić and others
flavonoids as solvent (highest both SE and MAE. MAE 2013)
yields), MP: low (320 W was better than UAE
for 1 min for and SE with reduced
flavonoids), high consumption of solvent
(800 W for 5 min for and time
total phenolics)
Wheat UAE Bran Flavonoids 64% ethanol at 333.15 K 25 min Similar or better recovery (Wang and others
in ultrasonic cleaning rate 2008cc)
bath at 40 kHz F and
250 W UP, respectively)
Maritime pine SFE Bark Flavonoids CO2 + Ethanol as solvent 90 min SFE extract yield is (Braga and others 2008)
(catechin and and modifier (10%, comparatively higher
epicatechin) v/v), 30 MPa Pc , static than that of
extraction (10 min) and hydro-distillation. Rapid
dynamic extraction (90 and efficient recovery in
min) at Tc 323.15 K shorter extraction time
(Continued)

Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 13
 Table 3–Continued.

Green extraction Plant Target phenolic Optimum extraction

Plant sample technique matrix/part compound parameters Extraction time Remarks Reference
Dittany of crete MAE Stem Phenolic Solvents (methanol, 1 min MAE with acetone as (Proestos and Komaitis
compounds acetone, ethyl acetate, solvent gives maximum 2008)
20 mL of each) 750 W yield of thermolabile
MP for 1 min polyphenols, better
than CSE in short time
intervals with less
solvent consumption
Grape bagasse SFE Stems, skins and Anthocyanins, 20 g of bagasse as feed 300 min 20 MPa gives efficient, (Farı́as-Campomanes and
(Piso) seeds catechins, material, CO2 + 96% rapid, and enhanced others 2013)
glycosides of ethanol 10% (w/w) as recovery of phenolic
flavonols modifier at Tc (313 K), compounds
2 extraction cycles at Pc conventional SE
20 and 35 MPa with extraction technique
Polyphenols extraction by green methods . . .

S/F ratio 80 and 115,

respectively
Apple PLE Pulp and peel Catechins, 99% methanol (solvent), 5 min (static Comparable recovery with (Alonso-Salces and others
flavonols 313.15 K temperature, mode) reduced solvent 2001)
(quercetin) and 7 MPa pressure amount, handling, and
anthocyanins time required than CSE
Jabuticaba (Plinia PLE Skin Anthocyanins Extractor conditions: 9 min (static Higher recovery: 2.15-fold (Santos and others 2012)
cauliflora) Pressure (5 MPa) and mode) anthocyanins (13%)
553 K temperature and 1.66-fold (8%)

14 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017
Guava (Psidium MAE Leaves Flavonoids Ionic liquids (1-Butyl-3-
guajava) methylimidazolium
chloride ([bmim]Cl),
1-butyl-3-
methylimidazolium
tetrafluoroborate
([bmim][BF4 ]) (20 mL
of each ionic liquid) at
343.15 K temperature
Coffee SFE Grounds and husk Phenolic Pc of 20 MPa (husk) and
compounds 10 MPa (spent coffee),
4% and 8% ethanol
total phenolic
compounds than CSE at
lower temperature
10 min Efficient extraction of (Du and others 2009)
phenolic compounds
with relatively excellent
absorbing abilities of IL
solutions used for MAE
process as compared to
traditional reflux
extraction
60 min (husk), High extract yield, that is, (Andrade and others
60 min (spent 15 ± 2% for spent 2012)
coffee) coffee grounds with


(w/w) as solvents, Tc
323.15 K (coffee husks)
and 333.15 K (coffee
grounds)
PLE Flakes (glycone of apiin Temperature (313.15 K),
Parsley(Petroselinum and pressure (7 MPa),
crispum) melonyl-apiin particle size (<850
µm), S/F ratio (250)
and 75% flush volume
ethanol and 3.1 ± 4%
for coffee husks by SFE
for phenolic compounds
Static extraction Improved recovery of 6 (Luthria 2008)
(5 min) phenolic compounds
with wider solvent
choice without any
thermal degradation
(Continued)

C 2017 Institute of Food Technologists®

 
C 2017 Institute of Food Technologists®
Table 3–Continued.

Green extraction Plant Target phenolic Optimum extraction

Plant sample technique matrix/part compound parameters Extraction time Remarks Reference
Apple PLE Pulp and peel Catechins, 99% methanol (solvent), 5 min (static Comparable recovery with (Alonso-Salces and others
flavonols 313.15 K temperature, mode) reduced solvent 2001)
Polyphenols extraction by green methods . . .

(quercetin) and 7 MPa pressure amount, handling and

anthocyanins time required than CSE
Cabbage (Red) PHWE Leaves Anthocyanins 2.5 g (sample), 372.15 K 7 min Fast recovery and (Arapitsas and Turner
at identification of 2008)
5 MPa solvent ratio: polyphenols coupling
water/ethanol/formic with HPLC-DAD
acid (94:5:1, v/v/v).
Bitter melon PHWE Fruit Chlorogenic acid, Methanol as solvent at 5 120 min Faster and high yield in (Budrat and Shotipruk
(Momordica genistic acid MPa and short time (2 h) as 2009)
charantia) and catechin 423.15-473.15 K with compared to SE (6 h)
2 mL/min of flow rate
Citrus (Citrus PHWE Peel Flavanones 1 cycle of PHWE at 433.15 10 min High yield Hesperidin (3.2 (Cheigh and others 2012)
unshiu) (hesperidin and K temperature and fold) Narirutin (3.7 fold)
narirutin) 10.13 MPa pressure than CSE
1 MP (Microwave Power).
2 SE (Soxhlet Extraction).
3 UP (Ultrasonic Power).
4 CSE (Conventional Solvent Extraction).
5 RE (Reflux Extraction).
6 S/F (Solvent-to-feed ratio).
7 F (Frequency).
8T (Critical temperature).
c
9P (Critical pressure)
c

Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 15
Polyphenols extraction by green methods . . .
Figure 5–Operational schematic principle and mechanism of pressurized liquid extraction (PLE) system.
solvents alone; for example, isopropanol and ethanol (Luthria and
others 2007; Mustafa and Turner 2011).
Matrix characteristics. The analyte recovery rate and extraction
efficiency of PLE is also affected by plant matrix characteristics.
Prominent factors in this regard include the nature of target com-
pounds, the relative bonding behavior of the analyte with the bi-
nary extraction solvent, and the particle size distribution and mois-
ture contents of botanical samples. These factors can affect the PLE
selectivity, thereby subsequently affecting extraction efficiency and
recovery rates of phenolic compounds from matrices (Mustafa and
Turner 2011). Molecule bonding behavior during solvation is af-
fected by matrix moisture contents, which are unique to every
plant. The characteristic particle size of matrix molecules affects
the final extraction yields of targeted components by influencing
mass transfer rate and extraction kinetics from various foodstuffs
or herbal preparations (Carabias-Martı́nez and others 2005).
Extraction time and temperature. Operational conditions of
temperature and pressure also significantly influence PLE selectiv-
ity and efficiency. As PLE involves use of elevated temperatures un-
der reduced pressure, the use of thermal energy helps to disrupt the
matrix structure by overcoming molecular bonding forces (Luthria
2008). Targeted phenolic compounds are present in bound form in
the sample matrix, and elevated temperatures are used to decrease
activation energy to overcome the interactive forces (cohesive and
adhesive) between matrix and solvent molecules to bring about
desorption. After wetting of the plant matrix is achieved by sol-
vation, elevated temperatures result in minimized surface tension
between samples, solvent, and solute interfaces during PLE. This
reduction in surface tension causes formation of solvent cavities
that permit dissolution of analyte in the solvent. The elevated
temperature also improves extraction efficiency by decreasing ex-
tractant viscosity, which leads to improved penetration inside the
sample matrix (Wang and Weller 2006). Application of high pres-
sure is, however, reported to exacerbate the problems associated
with air-bubbling during the extraction process, which can lead to
16 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017
low solubility rates (Carabias-Martı́nez and others 2005; Mustafa
and Turner 2011).
PLE applications for the green extraction of polyphenols
A survey of the literature suggests that PLE has been gaining
popularity during the last couple of years as a green method for
polyphenol extraction from herbal preparations. This increasing
trend is attributed to PLE automation, which allows extraction in
shorter time intervals with a minimum solvent and sample pre-
treatment requirements (Garcia-Salas and others 2010; Mustafa
and Turner 2011). PLE has been successfully employed for optimal
extraction of anthocyanins from freeze-dried red grape skin using
acidified water as a solvent. Among 6 solvents, acidified methanol
was found to provide maximum recovery rates of anthocyanins
and total phenolics in extracts obtained by PLE at 333.15 K tem-
perature and 10.1 MPa pressure. The results show a considerable
decrease in the consumption of solvent and a total extraction time
of 3 min compared with the 20 min for SE. PLE at elevated tem-
perature has proved to be an efficient eco-friendly technique for
the extraction of anthocyanins and total phenolics from red grape
skin (Ju and Howard 2003).
PLE has also been optimized in order to gain a substantial re-
covery of polyphenols from apple peel and pulp. In this study,
the extraction of total phenolics content was optimized using dif-
ferent process variables (solvent, pressure, temperature, and static
time). Optimized conditions for maximum polyphenol recovery
were reported to be pure methanol as extractant at 313.15 K tem-
perature and 7 MPa pressure for 5 min under static mode. In
conclusion, the efficiency of PLE as a green technique for ex-
traction of polyphenols was found to be comparable with CSE,
with reduced consumption of solvent volumes (20 to 40 mL for 2
extraction cycles) and with less time required for sample prepara-
tion (Alonso-Salces and others 2001).
The skin of Jabuticaba, a Brazilian native plant, has been re-
ported to be a rich source of anthocyanins and antioxidants. An

C 2017 Institute of Food Technologists®
Polyphenols extraction by green methods . . .
optimization study was carried out using RSM to determine the
optimal PLE conditions for polyphenol extraction from Jabuticaba
skin. The independent variables were extraction temperature (313
to 393 K) and pressure (5 to 10 MPa) with extraction time of
3 to 15 min. After optimization, the authors indicated improve-
ments in anthocyanins (13%) and other phenolic compound (8%)
recovery rates as compared to the traditional percolation method
at reduced pressure. Optimized PLE process variables include 5
MPa pressure and 553 K temperature with 9 min of extraction
time under static mode. PLE resulted in an enhanced extraction
yield rate (13%) and total phenolic contents (7.8 mg GAE/g DW)
as compared to the yield rate (12%) and total phenolic contents
(4.8 mg GAE/g DW) achieved using conventional percolation.
This study highlighted the promising potential of PLE as an eco-
friendly and economically viable technique that can be used as an
alternative to traditional percolation (Santos and others 2012).
Similarly, in another study, PLE was used for optimized extrac-
tion of phenolic compounds (glycones of apiin and melonyl-apiin)
from parsley flakes of variable particle size subjected to different
parameters: temperature, pressure, and S/F ratio with static extrac-
tion time. The extraction efficiency of phenolic compounds was
compared using 2 binary solvent systems: 50:50 v/v (ethanol/water
and acetone/water). In addition to particle size and S/F ratio as sig-
nificant influential factors, the sample preparation step is regarded
as one of the most crucial factors affecting final yield rate. Flush
volume was found to affect extractant consumption significantly
in terms of waste production. PLE was concluded to be an ef-
ficient green extraction technique with maximum recovery rates
of phenolic compounds from parsley flakes using the following
optimized parameters: temperature (313.15 K), pressure (7 MPa),
static extraction time (5 min), particle size (<850 µm), S/F ratio
(250), and flush volume (75%) (Luthria 2008). Table 3 presents a
comparative overview of PLE for polyphenols in comparison with
other methods.
PHWE
PHWE is another popular green extraction method among
the various green extraction techniques. This water-based ex-
traction process has been described as appealing in the published
literature because of its ready and cost-free availability, nontoxi-
city, nonflammability, and acceptance as an eco-friendly solvent.
Nevertheless, dissolution of organic compounds such as polyphe-
nols in water has restricted its use as a widely accepted technique
(Ong and others 2006; Plaza and Turner 2015). However, elevated
temperatures bring about significant changes in physicochemical
characteristics, such as viscosity, surface tension, and dissociation
constant. These effects improve PHWE effectiveness as a green
extraction method with respect to selectivity for phenolic com-
pounds and reduction in extraction times (Hawthorne and others
2000; Cheigh and others 2012; Vergara-Salinas and others 2015).
The application of hot water in the PHWE technique dates back to
the 1990s with the pioneering work of Hawthorne and coworkers
regarding environmental samples, and it is also regarded as sub-
critical water extraction, superheated water extraction, or ASE
employing water as an extractant. Pressurized water is used at a
temperature range operating above boiling point and below the
critical point of water, which are 273 K at 0.1 MPa and 647 K at
22.1 MPa pressure, respectively (Plaza and Turner 2015; Vergara-
Salinas and others 2015). The type of instrumentation employed
for PHWE with pressurized hot water (PHW) as extractant is, for
practical purposes, the same as that for PLE, illustrated in Figure

C 2017 Institute of Food Technologists® Vol. 00, 2017 r Comprehensive Reviews in Food Science and Food Safety 17
5. The advantages, disadvantages, and limitations of PHWE are
presented in Table 1.
Extraction principle and mechanism. The extraction mecha-
nism of PHWE consists of 4 steps that take place sequentially in
an extractor chamber filled with proportionate quantities of sand
and plant sample material. The 4 steps are as follows: (1) solute
desorption from multiple active sites on the matrix surface; (2)
diffusivity of pressurized water into the matrix material; (3) so-
lute partitioning from matrix molecules into the extractant; and
(4) solute elution to the collection vessel from the extraction cell.
An earlier study has described the PHWE mechanism as a phe-
nomenon compatible with a thermodynamics model. This model
advocates that extraction of phenolic compounds from plant ma-
trices by PHWE is a 2-stage extraction process: (1) desorption of
compounds from the respective binding sites on or in the sample
matrix by facilitated diffusion, and (2) elution of the eluent (target
compound) from the sample based upon a thermodynamic parti-
tioning coefficient (KD) comparable to elution chromatography.
Accordingly, it is noted that the extraction of phenolic compounds
is governed by various factors, such as diffusion rate, solubility,
equilibrium of the desorbed compounds in the sample matrix, and
also extraction mode (static or dynamic) conditions (Rodriguez-
Meizoso and others 2006; Teo and others 2010; Vergara-Salinas
and others 2015). PHWE utilizes pressurized water of variable po-
larities under controlled conditions of temperature (273 to 647 K)
and pressure (0.1 to 22.1 MPa), as the polarity of water tends to be
close to that of organic solvents such as alcohols. This is the main
reason for reduced usage of organic solvents and making PHWE
a suitable green method for the extraction of polyphenols from
plant matrices (Plaza and Turner 2015).
Factors influencing PHWE efficiency
The main factors affecting PHWE efficiency with respect to
selectivity and recovery rates of phenolic compounds include the
aqueous solubility of polyphenols, pressure, temperature, extrac-
tion time, flow rate, and adjunct additives or modifiers.
Aqueous solubility of phenolic compounds. PHWE efficiency
is reported to be affected by changes in the aqueous solubilities
of various phenolic compounds inside the extraction cell dur-
ing the PHWE process. Specifically, aqueous solubility influences
PHWE efficiency by disturbing mass transfer rates occurring dur-
ing the first stage of the PHWE process. During this stage, there
is the possibility of solute removal until total solubilization of so-
lute with extractant inside the vessel (Srinivas and others 2010).
Aqueous solubility is not affected by high pressures due to the sig-
nificant incompressibility of water molecules under the prevailing
conditions of elevated temperatures and pressures. As described
earlier in the extraction mechanism section, the solubility of so-
lutes is temperature-dependent. The dielectric constant of water
is reduced due to the weakening of intermolecular interactions,
that is, H2 -bonding within water molecules. The dielectric con-
stant is 80 at ambient room temperature, which decreases to a
value of 27 (near to that of organic solvents such as methanol and
ethanol at 298.15 K) at 5 MPa pressure and 523.15 K of tempera-
ture during the PHWE process. Hence, the aqueous solubility of
PHW is increased at temperatures above 373.15 K by permitting
dissolution of a variety of hydrophobic compounds, making it a
favorable solvent for green extraction (Briones-Labarca and others
2015; Vergara-Salinas and others 2015). Srinivas and others (2010)
reported an exponential rise in the aqueous solubility of polyphe-
nols with a gradual increase in temperature during the PHWE
Polyphenols extraction by green methods . . .
procedure. This leads to enhanced mass transfer and diffusion rates
resulting in higher efficiency.
Effect of elevated temperature and pressure on selectivity. The
extraction efficiency of PHWE is also influenced by diffusivity of
the target phenolic compounds. Elevated temperatures alter ex-
tractant polarity and generally increase solubility rates to a higher
extent, leading to enhanced polyphenol extraction (Teo and oth-
ers 2010; Plaza and Turner 2015). However, high temperature
has some inevitable consequences such as thermal degradation of
thermolabile phenolic compounds. This necessitates further clean-
up after PHWE due to the presence of unwanted contaminants.
Lower selectivity at high temperature during PHWE is a potential
cause of unwanted components along with targeted polyphenols
extracted from a wide variety of food materials (Srinivas and others
2010).
In summary, careful optimization of extraction temperature is
important in PHWE, in terms of gaining enhanced solubility of
phenolic compounds with maximum mass-transfer kinetics and
minimum degradation. For example, PHWE resulted in enhanced
extraction of flavonoids from yellow Thai silk waste at a tempera-
ture range of 323.15 to 352.15 K in comparison with PLE at the
same temperature using ethanol as an extractant (Vergara-Salinas
and others 2015).
Flow rate
High water flow rate in a continuous manner suppresses chemi-
cal reactions during PHWE operation. Sufficiently high and opti-
mized flow rates will decrease the retention times of target analytes
at elevated temperatures, with enhanced recovery of polyphenols.
Flow rate also helps to prevent the kinetics being limited by the
characteristic aqueous solubility of phenolic compounds during
PHWE. High flow rates above the optimum will cause excessive
extract dilutions and will necessitate an additional concentration
step after PHWE (Plaza and others 2013; Briones-Labarca and
others 2015). For example, Liu and others (2013) have reported
an optimum flow rate of 4 mL/min for obtaining maximum an-
thocyanin recovery from red onion by employing PHWE. They
also reported degradation of the targeted analyte with lower quan-
titative yields due to an increase in continuous flow rate above the
optimum level.
Modifiers and additives
Modifiers are added in order to achieve higher PHWE process
efficiency and enhanced recovery rates of target compounds. The
solubility rate of polyphenols in PHW increases due to the addi-
tion of certain modifiers (organic or inorganic) and additives. The
reason for this increase is attributed to an alteration in the physic-
ochemical properties of PHW at high temperature. This results
in improved recovery of phenolic compounds under static and
dynamic modes of PHWE (Plaza and Turner 2015). For instance,
PHWE using a mixture of extracting fluids and ethanol (5%) has
resulted in an improved extraction yield of anthocyanins from red
cabbage (Teo and others 2010).
PHWE applications for the green extraction of polyphenols
PHWE as a green extraction technique has gained wide repu-
tation as a feasible alternative to conventional extraction methods
for polyphenols extraction from different plant matrices. The per-
tinent attractive features making this technique a preferred choice
include temperature-dependent selectivity, low operational cost,
and rapid operation. The prominent feature is the nontoxicity of
PHW as an extractant instead of toxic and expensive organic sol-
18 Comprehensive Reviews in Food Science and Food Safety r Vol. 00, 2017
vents for extraction purposes (Vergara-Salinas and others 2015).
Budrat and Shotipruk (2009) have compared the extraction effi-
ciencies of different polyphenols (chlorogenic acid, genistic acid,
gallic acid, and catechin) from bitter melon (Momordica charantia)
by employing PHWE and traditional techniques: methanolic ex-
traction and SE with aqueous methanol (MeOH). In the case of
PHWE extracts, positive correlation was reported between in-
creasing temperature and total phenolic content, and a negative
correlation for antioxidant activity with rising temperature. Specif-
ically, at 473.15 K, PHWE has resulted in significantly higher re-
covery rates of extracts rich in total phenolic contents (52 mg
GAE/g DW) as compared to the recoveries achieved with MeOH
extraction (6 mg GAE/g DW) and SE with aqueous methanol
(6.6 mg GAE/g DW). Antioxidant activity was also found to be
3 times higher in PHWE extracts as compared to other conven-
tionally obtained extracts. Minimal solvent consumption has been
reported for PHWE (2 mL/min) with a shorter extraction time
of 1 h compared to that required for MeOH extraction (200 mL,
4 h) and SE (200 mL, 2 h). In another instance, a similar re-
port has been published with regard to the improved extraction
yield of phenolic compounds (hesperidin and narirutin) obtained
from citrus (Citrus unshiu) peel (a byproduct of the citrus indus-
try) using PHWE. PHWE was proved to be more efficient and
attractive in terms of flavanone recovery and antioxidant activities
of PHWE extracts compared to SE and ME using ethanol and
methanol as extractants, respectively. The authors reported 1.9-,
3.2-, and 34.2-fold higher extract yields from PHWE in compari-
son with CSE using ethanol, methanol, and hot water, respectively
(Cheigh and others 2012). In another study, the PHWE process
for phenolic compounds from apple pomace was optimized us-
ing RSM. Using RSM, authors have optimized the extraction
conditions for obtaining maximum yields of flavonols from cider
byproducts. They reported optimal extraction yield of antioxidant
compounds at 393.15 K temperature and 3 min of extraction time
using PHWE (Plaza and others 2013).
Leaves of oregano (Origanum vulgare L.) are noted for being
rich in phenolic compounds, particularly polyphenols from fla-
vanone and dihydroflavonol subclasses. Selective recoveries of phe-
nolic compounds from oregano leaves have been carried out using
PHWE at a temperature range of 298.15 to 473.15 K and 15 min
extraction time. The leaf extracts from PHWE were subjected to
diode array detector (DAD)-based detection by HPLC-DAD for
polyphenol identification and quantification. Lower temperature
significantly improved the extraction of relatively polar compounds
(flavanone and dihydroflavonol) in a preferential manner. Flavonols
were found to be present in the form of quercetin with relatively
lower amounts of flavones. It was also noted that a gradual rise in
temperature up to 473.15 K resulted in increased extract yield (54%
on a DW basis) of less polar phenolic compounds (Rodriguez-
Meizoso and others 2006). The potential for industrial scale-up of
PHWE for nutraceutical production has been suggested in vari-
ous published reports (Rodriguez-Meizoso and others 2006; Liu
and others 2013; Plaza and others 2013; Plaza and Turner 2015;
Vergara-Salinas and others 2015). Table 3 presents a comparative
overview of PHWE for polyphenols in comparison with other
green methods.
Conclusion and Future Perspectives
Undoubtedly, useless and waste plant residues from vari-
ous processing industries may serve as an excellent source of
plant-derived polyphenols as natural antioxidants. Traditional
methods have been shown to be exhaustive, laborious, and

C 2017 Institute of Food Technologists®
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