Trends in Food Science & Technology 116 (2021) 975–991

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Trends in Food Science & Technology

journal homepage: www.elsevier.com/locate/tifs

Ultrasonication - A green technology extraction technique for spices:

A review
Madaraboina Venkateswara Rao a, Animesh Singh Sengar a, Sunil C K a, *, Ashish Rawson b, **
a
Department of Food Engineering, Indian Institute of Food Processing Technology, Tamil Nadu, India
b
Department of Food Safety and Quality Testing, Indian Institute of Food Processing Technology, Tamil Nadu, India

A R T I C L E I N F O A B S T R A C T

Keywords: Background: Spices are rich source of naturally occurring bioactives and are used in different food applications.
Ultrasound-assisted extraction Major spice bioactives include essential oils, oleoresins, polysaccharides, phenolics, alkaloids, vitamins, and
Bioactives carotenoids. Conventional extraction of these bioactives has been associated with a high requirement of time,
Spices
solvent, and energy which diminishes the application.
Integrated technologies
Scope and approach: This review discusses and summaries the recent findings on UAE for extraction of bioactives
from spices. The concepts, mechanisms, factors affecting the sonication process, and their application in the
extraction of spice bioactives are reviewed. The integration of UAE with other emerging technologies, mainly
microwave-assisted and supercritical fluid (CO2) assisted extraction methods in the field of spice bioactives
extraction are also explored. A comparison of different optimization and modeling methods used for UAE of
spices are discussed and enunciate the gaps and possible future trend.
Key findings and conclusion: Acoustic cavitation generated during ultrasound treatment produces shock waves,
microjets, shear force, and sonochemical reactions causing plant cell erosion and pore formation. It enhances
mass transfer paving way for application of green solvents such as water. Further the Two-site kinetic model and
Peleg’s model are most versatile in explaining the UAE of bioactives from spices. Maximized recovery of bio­
actives, could be attained by selecting combination of technologies and process parameters for improved energy
efficiency reduced time and energy consumption.

1. Introduction alkaloids, glycosides, sulphur-containing compounds, essential lipids,

Spices are the fresh or dried aromatic products derived from different
parts of the plant source, involving roots, stems, whole grasses, leaves,
flowers, and fruits (Rawson et al., 2013; Teng et al., 2019). Since the
ancient times, spices have been added to the foods to improve the flavor,
color, and organoleptic properties. The commonly consumed spices
involve black pepper, cardamom, turmeric, ginger, ajowan, annatto,
nutmeg, fennel, anise, saffron, chili, garlic, fenugreek, onion, rosemary,
clove, celery seeds, sage, and thyme (Perussello, 2020).
Currently, there is an enormous demand in the global market for
natural bioactives which can be a replacement of synthetic chemicals for
the development of food, pharmaceutical, and cosmetic products (Gia­
cometti et al., 2018). Among the natural sources, spices are well known
for their naturally occurring bioactives that have been generally
recognized as safe (GRAS), which consists of phenolic compounds,
oleoresins, carotenoids, and vitamins. Bioactive compounds possess
several medicinal and therapeutic functions like antimicrobial, antiviral,
antihypertensive, anti-inflammatory, antidiabetic, antioxidant, anti­
lithogenic, antimutagenic, hypolipidemic/hypocholesterolemic and
anticarcinogenic activities, and the stimulation of digestive system
(Sharif et al., 2018). These physiological and pharmacological proper­
ties have drawn industrial attention to use spices as potential ingredients
in the development of either functional foods or nutraceuticals or active
food packaging (Muhammad & Dewettinck, 2017). Due to these prop­
erties, spices have been used in a food matrix as antioxidants, food en­
richments, flavoring agents, seasoning agents, coloring agents, fortifiers,
and preservatives, throughout the world especially in India, China, and
many other south eastern Asian countries (Rubió et al., 2013).
In past few decades, spices have been globally marketed in the form
of either whole spices or ground powders, or spice extracts. Majorly,

* Corresponding author.
** Corresponding author.
E-mail addresses: sunil.ck@iifpt.edu.in (S. C K), ashish.rawson@iifpt.edu.in (A. Rawson).

https://doi.org/10.1016/j.tifs.2021.09.006
Received 1 February 2021; Received in revised form 12 August 2021; Accepted 10 September 2021
Available online 12 September 2021
0924-2244/© 2021 Elsevier Ltd. All rights reserved.
M.V. Rao et al.
these spice extracts (i.e., bioactives) are used in the making of cheese,
soups, salad dressings, beverages, confectionery, meat and meat prod­
ucts, dairy products, and bakery products (El-Sayed & Youssef, 2019;
Melgar-Lalanne et al., 2017). Moreover, spice extracts serve as an
alternative to the applications of whole and grounded spices for
providing stability required in product formation, uniformity, flavor,
and also free from impurities and microbial contamination with
extended shelf life (Gavahian, Chu, et al., 2020). The varied spectra of
spices possess variety of antioxidant, antimicrobial, and antifungal
properties that help in stabilizing the oxidation process of lipids, pro­
teins, and pigments and play a major role in the improving the sensory
and nutritional characteristics of food products (Pateiro et al., 2018;
Rubió et al., 2013).
In order to recover spice essential compounds, extraction is the
principal operation that isolates and separates the essential oils, oleo­
resins, and bioactive compounds from whole or grounded spices fol­
lowed by purification of crude extracts (Khadhraoui et al., 2019). Some
of the well-known methods for extraction are solvent extraction, me­
chanical expelling, hydrodistillation, steam distillation, maceration,
supercritical fluid extraction, ohmic extraction, and microwave extrac­
tion (Arya & Kumar, 2021; Gouda et al., 2021; Jiang et al., 2021;
ŠicŽlabur et al., 2021). However, recovery of spice extracts through
these methods have limitations such as high extraction time, low yield,
degraded quality, extra solvent requirement, loss of volatile compounds,
and high energy consumption in solvent extraction, mechanical expel­
ling, hydrodistillation, steam distillation, maceration; large capital in­
vestment in supercritical fluid extraction; electrode corrosion, thermal
effects and contamination of metal ions in ohmic extraction; and
requirement of the aqueous phase in microwave-assisted extraction
(MAE) (Gavahian, Sastry, et al., 2020; Rawson, Tiwari, et al., 2011;
Sánchez-Camargo et al., 2020; Sengar et al., 2020; Sunil et al., 2018).
Hydrodistillation is a highly efficient technique for extraction of ther­
mally stable components where system performs extraction through
boiling of water at atmospheric pressure. Although there are various
parameters (yield, extraction time, CO2 rejection, etc.) for comparison,
however, energy consumption per unit yield is the most appropriate
index to determine the comparative effectiveness of the extraction
process. Chen, Zhang, and Yang (2020) compared extraction of 1 g of
cinnamon oil through hydrodistillation and ultrasound assisted
Fig. 1. Comparison of different conventional and novel extraction methods for spice bioactives.
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Trends in Food Science & Technology 116 (2021) 975–991
hydrodistillation technique and observed that required energy for same
amount of yield was 1.49 kWh and 0.79 kWh, respectively. Lucchesi
et al. (2004) compared the hydrodistillation with solvent free micro­
wave technique for essential oil extraction from basil, garden mint, and
thyme and reported higher energy consumption, in case of hydro­
distillation (4.5 kWh) than solvent free microwave extraction (0.25
kWh). Likewise, solvent extraction has higher solvent requirement and
may increase the toxic level of the resultant volatile extract (benzene
and dichloromethane) (Roohinejad et al., 2017, pp. 21–55). However,
supercritical fluid extraction and pulsed electric field assisted extrac­
tions of volatiles are uneconomical (higher installation and operational
cost), limited operation capacity and time consuming processes (Roo­
hinejad et al., 2017, pp. 21–55) (Fig. 1).
Compared to these methods, UAE has advantages such as low-
temperature extraction, less time and energy requirement, moderate
capital, and quality retention of the extracts (Arya & Kumar, 2021).
Studies suggest that a moderate increase in temperature during ultra­
sound treatment could enhance the extraction efficiency, however a
further increase in temperature, could have a negative effect on
extraction efficiency and extract quality (Chemat et al., 2017; Li et al.,
2021). Ultrasonic high-intensity sound wave creates driving mechanism
for extraction of bioactive compounds, essential oils, and oleoresins
from spices. SEM images illustrate the effect of ultrasonic wave induced
cell disruption in the plant tissues through physical forces that are
developed during acoustic cavitation which help in the release of
extractable components in to the solvent within a short time by
improving the mass transfer rate (Chemat & Khan, 2011) (Fig. 2).
Additionally, Wu et al. (2015) have reported that ultrasonic disruption
of yeast cell begins with the cell wall causing release of cell wall poly­
saccharides, followed by cell membrane breakdown.
Ultrasonication is considered as a green technology due to its po­
tential to produce products free from environmental pollutants.
Extraction of essential compounds using ultrasound has proven to be an
efficient method that reduces the use of toxic chemicals. As toxic sol­
vents could be replaced by GRAS solvents since UAE provides wider
range of solvent selection, less energy requirement and a compact sys­
tem with ease of transferability. Moreover, with increasing consumer
awareness, it is the need of hour to produce a product with clear
ingredient label and no added chemicals (McDonnell & Tiwari, 2017).
M.V. Rao et al.
Fig. 2. Plant cell disruption due to acoustic cavitation (Adapted from Chemat and Khan (2011)).
Ultrasonication of product is capable to attain the desired quality
through matrix modification, microbial load reduction, enhancing
extraction processes, and so on with no added extra chemicals. Other
non-food application of ultrasound includes treatment of sludge, water,
air purification, inorganic pollutant decomposition by formation of
oxidative radicals. It also simplifies the environmental analysis, by
reducing the analysis time, simplifying the procedure and providing
more accurate results (Sillanpää et al., 2011, pp. 1–21). Conventionally
used digestion techniques are long and complex, however, combination
of microwave and ultrasound irradiation process makes it easier, safer
and automated through which digestion, distillation and extraction
appears to be more promising. Ultrasonic solvent extraction method
indicates higher recovery (92%) of organochlorine pesticides from soil
with reduced extraction time (82%) and solvent consumption (67%)
compared to the conventional solvent extraction method (Tor et al.,
2006).
Ultrasound waves are successfully utilized in the extraction of
essential oils, oleoresins, curcumin and other bioactive compounds from
spice matrices (Fig. 3) (Jiang et al., 2021; Morsy, 2015; Muhammad
et al., 2021). The precise control over the factors such as parameters
(power, frequency, pulsation, particle size, extraction time, system type,
temperature, solvent, and liquid to solid ratio (LSR)), and matrix pa­
rameters can result in an optimum quality and quantity of extracted
components. The discrete, as well as combined impacts of these factors,
have been investigated by several researchers on the extraction of bio­
actives from plant sources. There are some good reviews regarding
ultrasound-assisted processing of spices (Teng et al., 2019), food and
natural products (Chemat et al., 2017; Medina-Torres et al., 2017; Zhang
et al., 2018) and recovery of phenolic compounds from vegetative
Fig. 3. Schematic representation of the ultrasound assisted extraction (UAE) of bioactives from spices.
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Trends in Food Science & Technology 116 (2021) 975–991
sources (Medina-Torres et al., 2017). However, a detailed review
focussing on all the aspects of ultrasonication as green technology for
extraction of bioactives from spices was not brought into light. Hence,
the current review intends to deliver a comprehensive and up-to-date
overview of the concept and mechanism, affecting factors, bioactives
extracted and optimization of extraction process from various spices
using UAE.
2. Concept and mechanism of UAE
UAE has been recognized as green, emerging and non-toxic tech­
nology as it enables the scope of using green solvents (GRAS) by
replacing conventionally used organic solvents. Moreover, chemical free
operation and no toxic residue production creates an environment
friendly approach satisfying the objective of clean and green extraction
process. Chemat et al. (2017) reported that the CO2 generation was in
the ratio of 32:18:1 for soxhlet extraction, maceration, and UAE,
respectively, highlighting UAE as clean and green technology. Lower
energy consumption and higher retention of heat labile components
compared to conventional extraction techniques are few other advan­
tages. The ultrasonic waves consist of a sequence of compression and
rarefaction cycles, which can be propagated through any medium (solid,
liquid, or gas) leading to the displacement and dislodgment of molecules
from their initial locations. Ultrasound proliferation through liquid is
largely know and used for various application such as cleaning,
extraction, modification, etc. Moreover, Zhang and Abatzoglou (2020)
has discussed the food application of ultrasound assisted drying, that
includes airborne propagation of ultrasonic vibrations. On the other
hand, ultrasound employed in cutting shaft propagates through solid to
M.V. Rao et al.
obtain accurate and sharp cut with minimized product loss (Bhargava
et al., 2020; Tiwari et al., 2021, pp. 39–65). Ultrasonication bubbles
could be of two types, stable bubbles and transient bubble, in which
transient bubble are of more interest as they produce sonochemical re­
actions in the food system. Though single bubble sonoluminescence are
also known to have long lifetime and ability of light emission and
chemical reactions on rupture (Yasui, 2018). These bubble volumes will
expand (rarefaction) and contract (compression) over many consecutive
periodic cycles until they become shape unstable to produce fragmented
daughter bubbles. Eventually these bubbles implodes or collapse
violently to produce sonoluminescence, high pressure (up to 1000 atm)
and temperature (up to 5000K) inside the medium, and the phenomenon
is known as ‘acoustic cavitation’, which is the primarily driven force of
extraction enhancement by UAE (Chen, Sun, et al., 2020; Kumar et al.,
2021; Kumari et al., 2017; Wen et al., 2020).
Ultrasonication creates negative pressure in the liquid system and
generates acoustic cavitation which appears as bubble since gases can no
longer be dissolved under negative pressure (Yasui, 2018). Acoustic
cavitation can induce the different phenomena of alterations in the
cellular tissues of plants, such as matrix fragmentation, cell erosion, pore
formation, increased absorption, shear force, and changes in swelling
index. Cavitation produces shock waves, microjets, shear force and
turbulence which in turn results in modification of plant matrix and
accelerate extraction. The shock waves are produced during rebounding
of bubbles after collapse (pressure waves radiated during expanding of
bubble overtakes previously collapsed bubble’s pressure waves).
Imbalanced pressure field around the bubble causes penetrating liquid
jet formation during ultrasonication process (Yasui, 2018). These in turn
causes fragmentation of cell wall matrix to drive higher solubility of
bioactives in the solvent as it decreases particle size, improves surface
area which consequently results in high mass transfer rates in the
boundary layers of plant matrix. This phenomenon may attribute to the
collision of accelerated inter-particles and generation of shockwaves.
The other is the erosion, which implodes the cavitation bubbles over the
surface of the plant matrix. This causes the localized damage to the
cellular tissues, and these eroded locations facilitate the more contact of
solvent leading to its enhanced extraction. Sonoporation occurs after
formation and implosion of bubbles which in turn generates the shear
Fig. 4. Effect of ultrasonic parameters and its mechanism of action.
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Trends in Food Science & Technology 116 (2021) 975–991
force and turbulence to accelerate release of bioactives. Acoustic
streaming are steady fluid motions generated due to high amplitude
sound waves while propagating through the fluid medium. Ultrasound
improves the swelling index and water absorption of plant matrix,
thereby increasing the diffusion and desorption of solutes to the solvents
resulting in enhanced extraction. Thus enhanced extraction yield by the
UAE cannot attribute to one mechanism, but due to all combinational
mechanisms (Fig. 4) (Bhargava et al., 2020; Chemat et al., 2017; Wen
et al. 2018, 2020). Oxidative radical formation during ultrasonication
are well known and includes (OH, O, H2O2 and O3), out of which OH are
dominant probably because O atom reacts with the liquid water at the
bubble wall to produce more of OH than other. Since
oxidation-reduction potential is much higher for OH radical (2.02 V)
than H2O2 (1.495 V), it plays an important role in sonochemical re­
actions (Yasui, 2018). However, production of oxidative radical depends
on the ultrasonication frequency and bubble temperature. Radicals were
produced lesser at temperature 7000 K compared to 5000 K, this could
be due to consumption of oxidation radicals inside the air bubbles by
oxidizing N2 at higher temperature (Yasui, 2018).
Also, the solvents used for treatment influence the ultrasonic effi­
ciency. For instance, the violent collapse of bubbles at higher tempera­
ture causes dissociation of methanol molecules (endothermic).
Increasing methanol concentration due to dissociation of methanol
molecules causes reduction in the bubble temperature. Presence of salt,
surfactant, sugar and alcohol above a transient concentration causes
retardation in bubble-bubble coalescence which generally occurs due to
attractive secondary Bjerknes forces. Coalescence could be completed
only after thinning and rupture of liquid film between the two bubbles,
but the solutes present in the medium increases solvent surface tension
which in turn inhibits the larger bubble formation. Subsequently,
acoustic cavitation leads to formation of tiny active bubbles in the liquid
medium and rarely the larger inactive bubbles. Thus, sonoluminescence
intensity improves with increasing solutes up to certain concentration.
In general, UAE has been employed in the plant matrix by using
instruments such as ultrasonic bath and ultrasonic probe, which are
based on the piezoelectric transducer as a source of ultrasound waves.
Ultrasonic bath and probe type sonicator are frequently used, to which
bath systems are economically sound and easy to operate, but its low
M.V. Rao et al.
reproducibility limits their use in various extraction processes because
of their limited generation of frequencies (either 20 or 40 kHz) (Medi­
na-Torres et al., 2017; Wen et al., 2018). On the other hand, ultrasound
probe-system makes direct contact with the medium through the im­
mersion of horn in the extraction vessel and release the ultrasound
waves in the extraction medium with minimal energy loss. The
probe-based ultrasound allows to generate a power up to 100 times more
than that obtained in the ultrasonic bath, and also the uneven energy
distribution and reducing power with prolonging time make the ultra­
sound sound bath less efficient as compared with probe systems.
3. Factors affecting the UAE process
3.1. Effect of ultrasound process parameters
3.1.1. Power
The cavitation effect and the erosion of the transducer depend on the
amplitude of the system, but high amplitude may not necessarily
enhance the cavitation and extraction performance because UAE mainly
depends on the other operational conditions such as target compounds
and type of spice (Zia et al., 2020). The ultrasonic power has been
broadly employed for the extraction of bioactives from spices and varied
in the range of 20–700 W (Kumar et al., 2021). Ultrasonication intensity
plays a major role in modification of plant cellular structure, with
increasing intensity it creates higher acoustic pressure and bigger size
bubbles which produces more violent collapse and leads to subsequent
chemical and physical reactions.
The extraction yield of UAE improves with increasing power density
up to the peak value and eventually decreases afterwards. These phe­
nomena of increments can be attributed to the increased disruptions and
pore formations in the cellular tissues caused by the generation of shear
forces, fragmentation, and localized pressures during the acoustic
cavitation, which results in the enhanced diffusivity and extraction
yield. However, with the increase in ultrasonic power, the number of
cavitation bubbles increases which leads to a large inter-bubble colli­
sion, deformation, and collapse in a non-spherical way and that may
decrease the impact of the bubble implosion. Besides, the increased
cavitation bubbles may surround the probe, hindering the energy
transmission to the extraction medium resulting in the decreased
extraction yield, also known as saturation effect. Further, the super­
heated localized temperatures and high free radical generation during
the implosion of the bubbles may also cause the degradation of bio­
actives and thus reduces the extraction yield (Chen, Sun, et al., 2020;
Kumar et al., 2021).
3.1.2. Frequency
Mostly frequency range (20–120 kHz) are involved in the extraction
of bioactives from spices (Kumar et al., 2021; Zia et al., 2020). The
high-frequency, low power intensity generates a large number of reac­
tive radicals in the extraction process, while low-frequency high power
density produces strong shear and mechanical forces (Kumar et al.,
2021). Radius of resonance and lifetime of a bubble are function of
frequency used for ultrasonication. With increasing frequency, bubble
size reduces and subsequently contains lesser energy compared to larger
bubbles. High energy collapse of bubble causes higher temperature at
molecular level and production of chemically active radicals through
dissociation of vapor. Selection of fixed low frequency might be due to
the phenomenon of generation of the lower number of cavitation bub­
bles with greater diameter favoring the stronger cavitation effect, which
decreases the cavitation impact with increasing frequency (Kumar et al.,
2021). Ultrasonic frequency and length of the rarefaction phase are
inversely related to each other. The larger intensities and amplitudes are
required at high frequencies to achieve the desired acoustic cavitation
and to lower the cohesive forces among the solvent and sample (Chemat
et al., 2017; Zia et al., 2020).
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3.1.3. Pulsation
The pulsation or duty cycle refers to a mechanism in which trans­
ducer periodically becomes ‘on’ and ‘off’. The impacts of varying duty
cycle on the extraction of bioactives from spices have been investigated.
The UAE operated in a pulsed mode reduces the formation of the number
of cavitation bubbles but improves the intensity of bubble collision and
that causes fragmentation in the plant tissue leading to improve
extraction until the equilibrium was reached (Chemat et al., 2017).
Further, pulsation reduces the overall energy used for extraction as well
as overheating of the ultrasonic equipment. Also, large degassing bub­
bles formed during continuous ultrasonic irradiation are considered as
vital problem in the acoustic field. Pulsed ultrasonication reduces the
large bubble formation to create more homogeneous acoustic field in the
liquid (Yasui, 2018).
3.1.4. Sonication time
The effect of varying ultrasound time on the extraction yield of
bioactives from spices have been extensively investigated. An increase in
sonication time enhances the yield initially, however, the bioactives
yield declines on further improvement in time (Zaimah et al., 2017).
Upon the initial increase in ultrasound time, the cavitation effect of the
sonication enhances the swelling, hydration, fragmentation, and pore
formation in the cellular tissue of the plant matrix (Sengar et al., 2020).
This causes release of bioactives into the solvent through the high mass
transfer rates and larger diffusivity of solvent into the matrix. The
intense structural damage to the solutes, inter-bubble collisions, and
saturation effect could be the reason for reduced bioactives extraction
yield under the ultrasound exposure for prolong time. Moreover,
continuous cavitation for prolonged time may cause degradation of
initially extracted compounds which are suspended or freely available in
the solvent.
3.1.5. Ultrasonication system type
The type of ultrasound system has a significant impact on the
extraction efficiency of bioactives from spices (Fig. 5). Jacotet-navarro
et al. (2015) compared the impacts of different types (bath, reactor, and
probe) of ultrasound systems on the extraction of phenolic acids (ros­
marinic, carnosic, and ursolic acids) from rosemary under identical
conditions of 40 ◦ C treatment temperature and 30 min treatment time.
Results suggest that ultrasound probe and reactor systems had the
almost similar total extraction yield of 18.8% and 18.1%, respectively,
while bath had the lower yield of 13.1% as compared to other systems of
ultrasound. Besides, the probe system had a higher yield of phenolic
acids (rosmarinic, carnosic, and ursolic acids) in the extract followed by
the reactor system, and finally, the ultrasound bath system. The higher
yield may attribute to the high power/intensity generation by
probe-based systems. Moreover, the cavitation effects of the probe-based
systems mainly depend on the tip diameter of the probe. The large
diameter probe generates the low cavitation effect in the extraction
medium, but the energy is distributed to a larger area, whereas a small
diameter probe has the greater cavitation effect, but the effect is
restricted to a narrow field. However, there is no investigation reporting
the effects of varying the tip diameters of the probe on the bioactives
extraction from spices. But the fixed diameters have been used such as
20 mm flat tip probe (horn) for ascorbic acid recovery from black
caraway seeds (Shaterabadi et al., 2020), curcumin extraction from
Curcuma amada (Shirsath et al., 2017) and Curcuma longa (Patil &
Rathod, 2020), 19 mm diameter probe for extraction of antioxidant
compounds from marjoram (Hossain et al., 2012), oleoresins from
nutmeg (Morsy, 2016) and essential oil from cardamom (Morsy, 2015),
13 mm and 3 mm diameter titanium probe for bioactives extraction from
Dedo de moca pepper (Dias et al., 2017) and polysaccharide from
fenugreek seeds (Kia et al., 2018).
Interestingly, Alexandru et al., (2013) carried out the pilot level UAE
(batch and continuous flow ultrasonic reactors) of phenolic compounds,
using as scaling parameter of 1 kg of clove and 20 L of ethanol as a
M.V. Rao et al.
Fig. 5. Different ultrasonic systems (a) ultrasound reactor, (b) ultrasound bath, (c) ultrasound probe.
solvent for the fixed exposure time of 45 min, which resulted in a higher
amount of total phenolic compound with a best antioxidant activity and
eugenol at continuous flow cycles of 1350 mL/min and power density of
700 W/L than the batch ultrasonic system at a power density of 18 W/L.
Furthermore, the flow ultrasonic reactor was coupled with multiple
(four) ultrasonic horns which were made of highly efficient pre-stressed
piezoelectric rings with a diameter of 50 mm. This large-scale experi­
ment elucidates that the type of ultrasound system can have significant
effect on extraction efficiency.
3.1.6. Temperature
In general, the impacts of varying temperature on the UAE yield of
bioactives from spices have been extensively investigated. The increase
in temperature initially enhances the UAE yield up to peak value and
further temperature rise causes degradation. The enhancing UAE yield
with increase in temperature could be due to the dual effect on both
solute and solvent where temperature increase on the one side improves
the solubility and desorption property of the solute in the solvent. While
on the other side it reduces the solvents viscosity and surface tension
through increasing vapor pressure which leads to the enhanced mass
transfer rates and solvent diffusivity in the plant cellular tissues. More­
over, further rise to high temperature may promote the larger degra­
dation rates of compounds in the UAE due to the weakened cavitation
effect as a result of enhanced shear stress, higher vapor pressure, and
lower surface tension of the cavitation bubbles (Chemat et al., 2017;
Kumar et al., 2021; Zia et al., 2020).
UAE at higher temperatures have also showed beneficial effect on
extraction yield. It resulted in the maximum extraction yield with higher
total phenols from wild garlic at elevated temperatures of 80 ◦ C while
raising the temperature from 40 to 80 ◦ C (Tomšik et al., 2016). This
phenomenon may be attributed to the rise in the number of cavitation
bubbles and also a larger solid-solvent contact, enhanced solvent
diffusivity with consequent improvement of desorption and solubility of
targeted compounds. However this effect was reduced when the tem­
perature reaches close to solvent’s boiling point (Chemat et al., 2017).
Interestingly, Zaimah et al., (2017) demonstrated that the concentration
and recovery of [6]-gingerol from ginger were enhanced with an in­
crease in temperature (from 35 to 55 ◦ C) at low frequency (28 kHz).
However, at the high frequency (800 kHz) the concentration and re­
covery have reached a maximum at 45 ◦ C and then slightly decreased
after reaching 55 ◦ C. Hence, the optimization of the temperature can
also be dependent on the other extraction parameters to obtain the
maximum yield of selected compounds with a prevention of heat labile
compounds, since this parameter can vary depending on the nature of
the product.
3.1.7. Particle size
Pulverization enhances the surface area and creates smaller particles
with ruptured cellular structure and intact cells. It is considered that
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Trends in Food Science & Technology 116 (2021) 975–991
ruptured cell structure leads to rapid extraction and causes initial rise in
extraction yield due to more availability and increased solvent contact
(Dassoff & Li, 2019). However, intact cells require higher energy input
for extraction as cell walls act as barrier to diffusion. Reduced particle
size minimizes the resistance to mass transfer as a result of reduction in
characteristic dimensions and disintegration of cellular structure.
Ultrasonication may cause instantaneous pressure drop during the pe­
riodic rarefaction and compression cycles, which occasionally result in
breaking of cells (Huang et al., 2018). It enhances the interaction be­
tween the solvent and target compounds and subsequently increases the
extraction yield.
3.1.8. Solvent type
The selection of solvent in UAE is a very crucial factor for extracting
different bioactives (i.e., polar and non-polar compounds) which is
primarily dependent on the solubility and polarity of targeted bio­
actives. Physical parameters including viscosity, surface tension, and
vapor pressure of the solvent are important parameters. These physical
parameters are recognized to affect the acoustic cavitation and its
threshold (Zia et al., 2020). Acoustic cavitation bubbles in aqueous
surfactants are smaller compared to the bubbles formed in pure water,
since presence of surfactants, salts, alcohol and sugar hinders the bubble
coalescence (Yasui, 2018). However different solvents (i.e., ethanol,
methanol, acetone, alcohols, water, and so on with varied portions of
water) have been used in the UAE extraction of different bioactives from
spices.
Different solvents (acetone, methanol, ethanol, and water) have been
used in the extraction of Cinnamomum burmannii Blume oleoresin by
Muhammad et al. (2021), and concluded that ethanol have a higher
extraction yield than the other solvents. Gorgani et al. (2017) elucidated
that sequential microwave-UAE with ethanol as solvent resulted in a
higher piperine yield than the other organic solvents (acetone, meth­
anol, and dichloromethane). Moreover, Shirsath et al. (2017) also
observed the maximum curcumin yield with ethanol as compared with
methanol, acetone, and ethyl acetate. These results can be attributed to
the higher polarity, vapor pressure, and lower viscosity and surface
tension of ethanol among the other solvent. Also, the acoustic cavitation
takes place easily in the lower viscosity and surface tension solvents
which leads to a larger extraction yield.
In recent years, ionic liquids, which are unique green solvents have
attracted the growing attention in plant-based product extraction
because of their distinctive property. They offer chance for the simul­
taneous extraction of hydrophilic and lipophilic bioactives through an
anion exchange, hydrophobic interaction and hydrogen bonding. Ionic
liquids have several benefits over conventional organic solvents, such as
thermal stability, chemical stability, negligible vapor pressure, less
toxicity, low flammability, tunable viscosity, recoverability and solvat­
ing properties for both polar and nonpolar compounds. But, limited
investigations have been conducted on the ionic liquids based UAE of
M.V. Rao et al. Trends in Food Science & Technology 116 (2021) 975–991

bioactives from spices (Kou et al., 2018).
3.1.9. Liquid to solid ratio (LSR)
LSR indicates the amount of solvent (mL) used for extraction of
essential compounds from solute (g). It is one of the principal parameters
during the mass transfer as more solvent volume helps to fasten the
diffusion process in cellular tissues. The yield of UAE improves with
increasing LSR up to a certain level (maximum) and reduces on further
increase in LSR value. The cohesive forces among the molecules must be
suppressed by the negative pressure of the rarefaction phase to generate
the cavitation effects in a solution. However, in low LSR the solution
cannot possess the desired cavitation effect because of its highly viscous
nature. Moreover, with the initial increase of LSR, the concentration and
viscosity of the solution decreases and this leads to a stronger cavitation
effect in an extraction medium. The larger difference in the concentra­
tion improves the diffusivity and dissolution of the solute into the sol­
vent augmenting the extraction process. The ultrasound exposed to the
larger quantity of spices at high LSR causes more fragmentation, erosion,
and sonoporation. Thus, enhances the extraction yield through
improving the contact area between spice matrix and solvent. The
reduction in the extraction yield at very high LSR can also be attributed
to the increased cavitation effect resulting in degradation of the desir­
able solute itself (Kumar et al., 2021; Medina-Torres et al., 2017; Zia
et al., 2020). The other reason could be, with increasing solvent content
in the extraction system, effective ultrasonic intensity available for
extraction reduces.
Effect of all the parameters in the related studies are summarized in
Table 1.
3.2. Matrix properties
determining the extraction conditions. The solubility and stability of the
extracted compound in the selected solvent as well as the temperature of
the liquid medium can impact the extraction efficiency. Likewise, the
size of the cavitation bubbles also has an impact on the extraction effi­
ciency if the extraction system is a heterogeneous and complex porous
matrix. The particle size and plant varieties (mainly vary in structural
and matrix composition) are the other essential factors affecting the
extraction efficiency (Chemat et al., 2017; Zia et al., 2020). Majorly, the
impact of varying particle size and varieties on the UAE yield of bio­
actives from spices have been investigated. The particle size of the
product is directly proportional to the superficial surface area exposed to
the selected solvent. As it tends to be smaller, the final yield of UAE
extraction improves because of the larger surface area, higher mass
transfer rate, and reduced diffusional resistances. While the larger par­
ticle size limits the final yield of UAE because of lower surface area and
diffusivity. This phenomenon was observed in the extraction of curcu­
min from Curcuma amada (Shirsath et al., 2017), and [6]-gingerol from
ginger (Zaimah et al., 2017). On the other hand, Gorgani et al. (2017)
reported that piperine yield was enhanced by reducing the particle size
of black pepper from 0.30 to 0.15 mm, which corresponded to an
improvement of 118% but further it remained almost same when par­
ticle size was reduced to 0.105 mm. A similar trend was observed in the
extraction yield of star anise oleoresin, and these results can be attrib­
uted that smaller particle size powders might cause the adhesion be­
tween materials and then impede the dissolution of the targeted
compounds (Li et al., 2018). Many spice varieties have been studied for
UAE of oleoresins from hot chili pepper (Sricharoen et al., 2017) and the
extraction yield generally depends on the structure and targeted com­
pound composition in the selected variety of spices.

The properties of plant matrix and target compounds are essential in

Table 1
Effect of ultrasound parameters on extraction of essential compounds from spices.
Parameter Spice Treatment Condition Time Effect of factors References

Power Cinnamon 20 kHz; 100–500 W 10–60 min Essential oil yield: Power, 100–300W ↑ and Guanghui et al.
(Cinnamomum cassia) 400–500W ↓ (2020)
Power Star anise (Illicium 100–350 W; 20–70 ◦ C 10–60 min Oleoresin yield: Power, 100–264W ↑ (highest at Li et al. (2018)
verum) 264W, 19.96%) and decreased with increasing
power
Power Dedo de moça pepper 20 kHz; 800 W; 40 ◦ C; titanium probe 120 min Oleoresin yield ↑ with ultrasonic intensity 150–450 Dias et al.
(Capsicum baccatum (13 mm) W/cm2 (2017)
L.)
Power, frequency, S/ Mango ginger 22 kHz and 40 kHz; 130, 160, 190, 220 60 min Curcumin yield: Power, 250 > 190 220 > 160> 130; Shirsath et al.
L, temperature, (Curcuma amada) and 250 W; probe type (d, 22 mm); frequency, 22 KHz> 40 KHz; solvent, Ethanol > (2017)
particle size pulsation 5s ON:OFF methanol > acetone > ethyl acetate; S/L, 1/25 > 1/
45 > 1/35 > 1/55 > 1/15; temperature, 55 > 45>
35 > 25 ◦ C; particle size, 0.09 > 0.21> 0.85 > 0.106
Power, frequency, Piperaceae (Piper 25 kHz and 40 kHz (bath type); 100, 3–30 min Piperine yield: Power, 100–125 W ↑ (highest at 125 Rathod and
temperature longum) 125, 150, 175 and 200 W; 30, 40, 50, W) and 150–200 W ↔ (at 25 KHz); frequency, 25 Rathod (2014)
60 and 70 ◦ C. KHz> 40 KHz (at 175W); solvent, Acetone >
Ethanol > Hexane; S/L, 1/2.5–1/10 g/ml ↑ with
highest at 1/10 g/ml and 1/20–1/40 g/ml ↓; time,
3–18 min ↑ (highest after 18 min) and 18–30 min ↔;
temperature, 30–50 ◦ C ↑ (highest at 50 ◦ C) and
50–70 ◦ C ↔ (at 125W, 25 KHz, 1/10, ethanol
solvent)
Power, frequency, S/ Ginger (Zingiber 28 kHz and 800 kHz (bath type); 40, 15, 30, 45, [6]-Gingerol recovery: Power, 40 > 80> 60 W (800 Zaimah et al.
L, temperature, officinale Roscoe) 60 and 80 W; 1/10, 1/20, 1/30, 1/50 60 min KHz) and 40 > 60> 80 W (28 KHz) (at 45 ◦ C, 45 min (2017)
particle size g/ml; 35, 45 and 55 ◦ C; 0.30, 0.89 and 1/10 g/ml); particle size, 1.77 > 0.89> 0.30 mm (at
1.77 mm. 70 W, 28 KHz and 40 KHz, 15 min, 1/10 g/ml,
45 ◦ C); time, 15 > 45> 30 > 60 min (28 KHz) and 45
> 15> 60 > 30 min (800 KHz) (under parameters 70
W, 1/10 g/ml, 45 ◦ C); temperature, 35–55 ◦ C ↑ (28
KHz) and 35–45 ◦ C ↑ and 55 ◦ C ↓ (800 KHz)
Power, frequency, Ginger (Kaempferia 20 kHz and 38 kHz; 250 W/L; 10, 20, 30, Essential oil yield: Frequency, 20 KHz> 38 KHz; Fan et al.
temperature, galangal L.) 100–150 ◦ C; 2–12 MPa; 40, 50, 60 pressure, 2–10 MPa ↑ and 12 MPa ↔; time, 10–20 (2015)
pressure min min ↑ and 30–60 min ↓;
Power, pulsation Ginger (Zingiber 20 kHz; 28–30 W; pulsation 30 min [6]-Gingerol maximum yield: power 36 W, pulsation Varakumar
officinale) (30–100%) 40%, time 5min and further 10–30 min yield ↓ et al. (2017)

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4. Pretreatment for UAE of bioactives from spices
The pretreatment of spices has a significant effect on the UAE yield of
bioactives, such as dehydration techniques and milling. Spices could be
used for extraction either directly as fresh or in dried form. Mostly, the
dried spices are preferred over fresh since they are more stable, more
concentrated, and have low interference from moisture. The commonly
employed drying techniques for spices are sun drying, hot air drying,
shade drying, freeze-drying, infrared assisted drying, microwave-
assisted drying (Kurup et al., 2020; Manousi et al., 2019; Rawson,
Tiwari, et al., 2011; Sunil et al., 2017; Teng et al., 2019). The different
drying methods could have different effects on the bioactive extraction
yield depending upon phenomenon involved. For instance, Samani et al.
(2017) evaluated the different drying methods (ultrasound, infrared and
hot air drying) at temperatures of 40, 50, and 60 ◦ C on the extraction
yield of essential oil from Satureja bachtiarica and reported that the
maximum essential oil yield was achieved at 40 ◦ C. Additionally, the
ultrasound drying led to a higher essential oil yield among the other
drying methods. Further, these were pulverized for enhancing the sur­
face area, mass transfer rates, and diffusion of solvent in the plant ma­
trixes (Saxena et al., 2018). The dried spices can swell and hydrate in the
solvent, causing the pores size increment in cellular tissues and high
diffusion rates across cell walls leads to an enhanced extraction (Medi­
na-Torres et al., 2017). Spices can be defatted for the enhanced UAE of
bioactive polysaccharides and phenolic compounds before drying and
milling. Kia et al. (2018) defatted the fenugreek seed sample with
sequential reflux of n-hexane and 95% ethanol before the drying and
milling for the extraction of polysaccharides by using the UAE.
5. Application of UAE in the extraction of bioactives from spices
Spices are well known for their naturally occurring bioactive com­
pounds that have drawn industrial attention because of their medicinal
and nutritional properties. The majority of the bioactive compounds in
plants are produced in the form of secondary metabolites except for the
polysaccharides, dietary fibers, bioactive peptides, vitamins, minerals,
and bioactive lipids such as essential oil and oleoresins. These secondary
metabolites, also named phytochemicals, are classified into alkaloids,
terpenoids, phenolic compounds, carotenoids, and pigments (Kumari
et al., 2017). The UAE has been broadly employed for the extraction of
these bioactive compounds from different spices due to their high
extraction yields, short extraction time, less energy consumption, less
environmental impact, and also prevention of heat labile compounds
(Sánchez-Camargo et al., 2020).
5.1. Essential oils
Essential oils, also named volatile odoriferous oil, are the group of
volatile aromatic compounds that are produced in the form of secondary
metabolites by various parts of aromatic plant species such as barks,
buds, seeds, leaves, flowers, peels, and so on (Duarte et al., 2018, pp.
1–19). These volatile essential oils are concentrated liquid with a strong
odor that imparts the aroma to food, and thermally unstable and can be
degraded during the conventional extraction at a higher temperature.
The benefits of employing the UAE lie in the intensification of extraction
yield at low temperatures via cavitation which also preserves heat labile
compounds (Giacometti et al., 2018), and are summarized in Table 2(a).
For example, Guanghui Chen, Zhang, and Yang (2020) compared
hydrodistillation extraction with ultrasound-assisted hydrodistillation
(UAHD) extraction of essential oil from cinnamon bark. Results suggest
that UAHD intensified the 27% of oil yield (from 1.68% to 2.14%), and
also reduced the 50% of extraction time (from 120 min to 60 min) as
compared with hydrodistillation. Moreover, UAHD retained a higher
amount of vital trans-cinnamaldehyde compound (81.9%) in the
extracted essential oil than that of hydrodistillation (78.3%). Similarly,
Jadhav et al. (2020) also reported that UAHD induced the high extrac­
tion yield of cinnamon bark essential oil (3.17%) with a higher amount
of oxygenated compounds (96.32%), and reduced extraction time (35
min) than that of hydrodistillation induced extraction yield (2.98%),
oxygenated compounds (81.32%), and extraction time (180 min).
Furthermore, Morsy (2015) obtained higher essential oil yield (7.4%)
from cardamom with an increased ratio of α-terpinyl acetate/1,8-cineole
contents (1.6:1) in oil under ultrasound probe treatment at a power of
30 W for 30 min followed by hydrodistillation as compared with
hydrodistillation-alone in Clevenger apparatus (7.05% of yield and
1.13:1 of ratio) for 360 min. Additionally, Kowalski (2015) reported a
significant improvement in essential oil yield of the mint leaf
(1.32–1.46%) and marjoram herb (1.13–1.27%) but not on chamomile
flowers after ultrasound-assisted water maceration treatment and this
may be attributed to the nature of product modified by UAE.

Table 2. (a)
Optimized conditions of ultrasound-assisted extraction (UAE) of essential oils from spices.
Spices Extraction variables Treatment Conditions Optimized conditions for Optimization Yield References
UAE/Major findings method (%)

Clove (Syzygium T:32–52 ◦ C; t: 30–60 min; US: bath type; F: 53 kHz; PS: < 0.5 mm; S: T: 60 ◦ C; t: 45 min; PC: Central composite 22.80% Tekin et al.
aromaticum) PC: 3–7% ethanol 5% response surface (2015)
design
Cardamom P: 10% (30 W) & 20 (60 US: probe type; LSR: 12:1; T: room P: 20%; t: 10 min NA 7.40% Morsy (2015)
(Elettaria W); t: 15 & 30 min temperature; S: water
cardamomum L.)
Cinnamon P: 300–600 W; t: 15–40 F: 20 kHz; P: 600 W; US: probe type; T: Solid loading: 25 g; Taguchi models- 3.17% Jadhav et al.
(Cinnamomum min; solid loading: 15–40 50 ◦ C; PS: < 100 μm; S: water solvent quantity: 100 ml; Orthogonal L16 (45) (2020)
cassia) g; solvent quantity: P: 600 W; t: 35 min array method.
100–400 ml
t: 10–60 min; P: 100–500 F: 25 kHz; S: water; US: ultrasonic cell t: 35 min; LSR: 7:1; ET: Taguchi models- 2.14% Chen, Zhang,
W; ET: 15–120 min; LSR: pulverizer 60 min; P: 300 W Orthogonal L16 (45) and Yang
4–12:1 array method. (2020)
White pepper NA LSR: 1:10; T: 100 ◦ C; ET: 7 min; P: 50 W: UAE yield was lower than NA 4.10% Wang et al.
(Piper nigrum L.) microwave power: 100W; PS: 40 mesh microwave-assisted (2018)
extraction
Ginger (Kaempferia Pressure: 2–14 MPa; T: US: ultrasound-assisted subcritical water Maximum yields at NA 2.58% Fan et al.
galangal L.) 100–150 ◦ C; ET: 10–60 extraction; S: water; evaluated ethyl trans- T:120 ◦ C; ET: 20 min; (2015)
min; F: 20 & 38 kHz; P: p-methoxycinnamate retention in Pressure: 10 MPa; P: 250
0–250 W/L essential oil extract W/L; F: 20 kHz

(Where, T = Extraction temperature (◦ C or K); US: ultrasound system type; t = ultrasonic time (min); F= Frequency (kHz); S = Solvent; P = Power intensity (W/cm2)/
Power (W)/Amplitude (%)/Power density (W/mL or L); DC = duty cycle (%); LSR = Liquid to Solid Ratio (mL.g− 1); PS: particle size (mm or μm) powder granularity
(mesh); SC: ethanol concentration (%); PC: plant concentration (%); ET: extraction time; NA-Not available)

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Tekin et al. (2015) reported that increase in extraction yield during
UAE could be due to rise in extraction temperature which subsequently
causes higher solvent vapor pressure. Moreover, it may cause
improvement in acoustic cavitation, which resulted in the high extrac­
tion yield of essential oil from clove at a frequency of 53 kHz (5% of
plant concentration) at 65 ◦ C and 45 min. Moreover, Fan et al. (2015)
reported that ultrasound-assisted subcritical water extraction intensified
the amount of ethyl trans-p-methoxycinnamate in the essential oil from
Kaempferia galangal L. at the optimized conditions of time 20 min,
pressure 10 MPa, power density 250 W/L, and frequency 20 kHz.
Therefore, the high extraction yields with greater retention of biological
activity by ultrasound-assisted subcritical water extraction makes it a
potential technology for industrial adaption. However, there is a need
for efficient optimization of type of extraction modes (either static or
dynamic) and process parameters (solvent flow rate, pressure, ultra­
sound parameters, and temperature) on bioactives extraction from
different spices.
5.2. Oleoresins
Oleoresins are the naturally existing mixtures (consists of resins and
essential oils) extracted from different spices with organic solvents. The
solvent type impacts the quantity and quality of the oleoresin extracts
(Said et al., 2015). These extracts can also be termed as “true essence” of
spices that impart flavor/taste and aroma to the foods, which highly
withstand the processing temperatures, and microbial contamination as
compared with essential oils due to presence of nonvolatile constituents
(such as resins, waxes, and fats) (Morsy, 2016; Shahidi & Hossain,
2018). UAE has been employed for the extraction of oleoresin from
different spices represented in Table 2(b), such as capsicum (Fernán­
dez-Ronco et al., 2013; Melgar-Lalanne et al., 2017), cinnamon
(Muhammad et al., 2021), nutmeg (Morsy, 2016), ginger (Said et al.,
2015; Supardan et al., 2012), and star anise (Li et al., 2018), to overcome
the shortcomings of traditional extraction methods.
Muhammad et al. (2021) reported that UAE resulted in the higher
oleoresin extraction yield, total phenolic content, and flavonoid content
of cinnamon than the traditional method based on the solvent type (such
as acetone, methanol, ethanol, and water). Additionally, UAE with
methanol solvent increased the recovery (μg/g dry material) of phyto­
chemicals such as cinnamic acid (828.3–934.2), protocatechuic acid
(193.1–227.8), procyanidin B2 (984–1396), catechin (14.9–51.1), epi­
catechin (15.6–52.5), 3,4-dihydroxybenzaldehyde (1078–1138) except
the quercitrin compound (16.1–13.23), as compared with traditional
extraction method. Moreover, Supardan et al. (2012) reported that ul­
trasound bath operated with a frequency of 42 kHz, extraction tem­
perature of 60 ◦ C resulted in 1.75 times more extraction rate than the
soxhlet extraction by using the ethanol solvent. Said et al. (2015) re­
ported that UAE induced 1.75 times faster extraction rate of ginger
oleoresin than the soxhlet extraction. Additionally, UAE resulted in the
23.89% of star anise oleoresin yield with a 90.91% of trans-anethole
content, and this unpurified oleoresin extract has exhibited a greater
microbial inhibition effect against Escherichia coli and Bacillus subtilis
than a purified oleoresin (Li et al., 2018).
Morsy (2016) reported that UAE with an ethanol ratio of 1:4 at a 40%
maximum output power for 10 min at room temperature resulted in a
similar nutmeg oleoresin recovery to that obtained in maceration after 3
days. In addition, oleoresins extracted by the UAE method exhibited
superior quality than the maceration in terms of β-pinene to myristicin
and safrole ratio, and sensory scores (such as clove-like attribute, spice
aroma, and sweet aroma). Interestingly, UAE also has the advantage of
obtaining the low solvent residues in oleoresins from a C. domestica
(16.00%) and C. xanthorrhiza (15.66%) rhizomes as compared with
soxhlet extraction (31.58% and 43.72%) and maceration extraction
(30.03% and 46.57%).
5.3. Phenolic compounds
Phenolic compounds are one of the primary phytochemicals that
impart the sensorial characteristics to the foods because of their anti­
oxidant, antidiabetic, anticancer, antiallergic, anti-inflammatory, and
antiviral properties. These phenolic compounds have an aromatic arene
(phenyl) ring with an attachment of at least a single hydroxyl (OH)
group. Based on the arrangement and number of carbon atoms, phenolic
compounds can be divided into subgroups such as polyphenols, phenolic
acids, flavonoids, stilbenes, lignins, and lignans. These compounds are
broadly extracted from various spices through UAE because of its ad­
vantages such as less solvent consumption with minimal impact on the
environment, short extraction time, and high penetration force (Oreo­
poulou et al., 2019).
All the principal parameters affecting the UAE efficiency of phenolic
compounds in terms of extraction yield and its quality, are represented
in Table 2(c). The UAE of polyphenols from ginger was carried out to
evaluate its antioxidant and antimicrobial properties (Murphy et al.,
2020). The author found that UAE induced the total phenolic and

Table 2. (b)
Optimized conditions of ultrasound-assisted extraction (UAE) of oleoresins from spices.
Spices Extraction variables Treatment Conditions Optimized Optimization Yield References
conditions for method (%)
UAE/Major
findings

Nutmeg P: 20% (60 W) & 40% (120 W); t: 10 & US: probe type; LSR: 4:1; S: P: 40%; t: 10 min NA 8.26% Morsy (2016)
(Myristica 25 min ethanol
fragrans)
Star anise S: petroleum ether (b.p. 30–60 ◦ C), NA S: ethyl acetate; PS: Taguchi models- 23.89% Li et al. (2018)
(Illicium petroleum ether (b.p. 60–90 ◦ C), 60–80 mesh; LSR: Orthogonal L16 (45)
verum) acetone, anhydrous ethanol, 60:6; t: 30 min; P: array method
cyclohexane, & ethyl acetate; PS: 264 W
10–100 mesh; LSR: 30:6–90:6; T:
20–70 ◦ C; P: 100–350 W; t: 10–60 min
Paprika T: 298, 318 & 338 K; LSR: 2:1–6:1; S: F: 40 kHz; P: 200 W; US: bath S: hexane; T: 298 K; Mixed factorial 3- 84.00% Fernández-Ronco
(Capsicum ethanol & hexane type LSR: 4.3:1 22 experimental et al. (2013)
annum) design
Ginger (Zingiber P: 28–65 W; DC: 30–100%; t: 5–30 min Ultrasound assisted three phase DC: 40%; P: 36 W: NA 6.40% Varakumar et al.
officinale) partitioning at pH 5; 5% (W/V) t: 5 min (2017)
solid loading; 10% (W/V)
ammonium sulphate; 0.5:1 ratio
of t-butanol to slurry
Cinnamon S: acetone, methanol, ethanol, & water F: 80 kHz; T: 30 ◦ C; t: 1 h; LSR: S: ethanol NA 29.80% Muhammad et al.
(Cinnamomum 10:1 (2021)
L.)

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Table 2. (c)
Optimized conditions of ultrasound-assisted extraction (UAE) of phenolic compounds from spices.
Spices Extraction variables Treatment Optimized conditions for UAE/ Optimization References
Conditions Major findings method

Ginger (Zingiber PC: 400–1200 mg/20 ml solvent; SC: 20–100%; T: US: bath; F: 35 The maximum total phenolic Central composite Murphy et al.
officinale) 30–70 ◦ C; t: 10–30 min kHz; P: 640 W; S: (1039.64 mg GAE/g of ginger response surface (2020)
ethanol extract) and flavonoid (492.57 ± design
3.5 mg QE/g of ginger extract)
contents at PC: 1200 mg/20 ml
ethanol, SC: 86%, t: 11min, & T:
65 ◦ C
Mango ginger S: ethanol, methanol, acetone & ethyl acetate; T: 25, DC: 50%; US: Maximum curcumin yield of 72% Peleg’s Shirsath et al.
(Curcuma 35, 45 & 55 ◦ C; LSR: 15:1–55:1; PS: 0.09–0.85 mm; probe type; ET: 1 was obtained at T: 35 ◦ C, LSR: 25:1, mathematical (2017)
amada) P: 130–250 W; F: 22 & 40 kHz h PS: 0.09 mm, P: 250 W, F: 22 kHz & model
S: ethanol
Cinnamon SC: 0–100%; t: 10–50 min PS: 40 mesh; US: Maximum total yield (0.76%), Central composite Lee et al. (2018)
(Cinnamomum ultrasonic Cinnamic acid (5.67 mg/100 mL) response surface
cassia) cleaner; S: and Cinnamaldeyde (205.26 mg/ design
ethanol 100 mL) was reached at SC:
55.34% & t: 33.12 min
SC: 0–96%; T: 40–80 ◦ C; ET: 20–60 min US: bath; F: 40 The maximization of total phenolic Central composite Cebi et al. (2019)
kHz; P: 172 W; S: content (TPC) of 149.3 mg GAE/g response surface
ethanol; LSR: dry weight was obtained on fuzzy design & Fuzzy
20:1 optimization with an SC: 72%, ET: modeling
50 min & T: 70 ◦ C.
41 and 2 mg/g dry weight of trans-
cinnamic acid and p-coumaric acid
contents of the extract resulted
Pepper (Capsicum S: water, acetonitrile, methanol, ethanol, acetone, US: bath; Maximum amount of capsiate Statistical mixture Vázquez-Espinosa
spp.) hexane & ethyl acetate; t: 5–15 min; T: 5–55 ◦ C; pH: P: 200 W (1323.68 μg/g) was extracted at S: design & Box- et al. (2019)
2, 5, & 8; LSR: 5:0.2–15:0.2 42% methanol + 58% ethyl Behnken response
acetate; t: 2 min; pH: 8; LSR: surface design
14.5:0.2; T: 60 ◦ C
Wild garlic T: 40–80 ◦ C; SC: 30–70%; t: 40–80 min; P: US: bath; PS: Maximum contents of extraction Central composite Tomšik et al.
(Allium ursinum 19.2–38.4 W/L 0.325 mm; LSR: yield (38.1%), total phenol (1.6 g face-centered (2016)
L.) 5:1; S: ethanol GAE/100 g dry weight (DW)), response surface
flavonoids (0.35 g CE/100 g DW) & design
antioxidant activity (0.71 mg/ml)
were obtained at T: 80 ◦ C, SC: 70%,
t: 79.8 min & P: 20.06 W/L
Fenugreek seed LSR: 10:1–50:1; t: 10–60 min; SC: 20–90%; US: bath; T: The maximum content of total Box-Behnken Das (2013)
(Trigonella extraction times (3 times of 50 min) 25 ◦ C; PS: < 0.5 flavonoid (16.22 mg/g) at LSR: response surface
foenum- mm; S: methanol 30:1, t: 50 min, and SC: 70% with 2 design
graecum) times of extraction time
Curry leaf P: 80–150 W; T: 40–80 ◦ C; SC: 40–80% LSR: 20:1; t: 20 Maximum extraction yields of Central composite Ghasemzadeh et al.
(Murraya min; S: methanol flavonoids such as catechin, response surface (2014)
koenigii L.) myricetin, & quercetin of 0.482, design
0.517 & 0.394 mg/g DW was
observed at T: 55.9 ◦ C, P: 145.49
W; SC: 80%
Ginger (Zingiber PS: 0.30, 0.89 & 1.77 mm; t: 15, 30, 45 & 60 min; P: Sonic assisted Maximum concentration and Linear & Zaimah et al.
officinale 40,60 & 80 W; LSR: 10:1–50:1; T: 35, 45 & 55 ◦ C; water extraction recovery of [6]-gingerol was polynomial model (2017)
Roscoe) SC: 0–15%; F: 28 kHz & 800 kHz (SAWE); observed at PS: 0.89–1.77 mm, t:
US: bath; S: 45 min, P: 40W, LSR: 30:1, F: 800
ethanol kHz, & SC: 10%.
High frequency (800 kHz) SAWE
gave a concentration and recovery
that was 2.69 times higher
compared to low frequency (20
kHz) SAWE
Lamiaceae PS: 0.3, 0.7 & 1.5; LSR: 10:1, 20:1 & 30:1; S: water F: 20 kHz; P: Maximum UAE yield of total 24& 23 Ðor et al. (2017)
(Thymus & ethyl alcohol 80%; T:25 ◦ C; polyphenol and flavonoid content experimental
serpyllum L.) SC: 30%, 50% & 70%; t: 5–90 min US: probe of 32.7 mg GAE/L & 16.7 mg CE/L design
at PS: 0.3 mm, LSR: 30:1 & S:
ethanol; SC: 50%
Dedo de moça P: 150, 300 & 450 W/cm2; T: 40, 50 & 60 ◦ C; S: US: probe; F:20 The recoveries of phenolics and Pseudo-first order Dias et al. (2017)
pepper ethanol & methanol kHz; P: 800 W; antioxidants increased with model
(Capsicum LSR: 20:1 ultrasound intensity, but higher
baccatum L.) ultrasonic intensities reduced their
yields
Marjoram Amplitude: 24.4–61 μm; T: 15–35 ◦ C; t: 5–15 min; S: P: 1500 W; F: 20 Maximized total phenol, Response surface Hossain et al.
(Origanum water kHz; LSR: 50:1; antioxidant activity, rosmarinic methodology (2012)
majorana L.) flow rate: 0.5 L/ acid, caffeic acid, carnosic acid,
min; US: probe and carnosol values in UAE extracts
were obtained at 61 μm amplitude,
T: 35 ◦ C & t: 15 min
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Table 2. (c) (continued )

Spices Extraction variables Treatment Optimized conditions for UAE/ Optimization References
Conditions Major findings method

Turmeric ILs: 1-butyl-3-methylimidazolium bromide Ionic liquid (IL) Maximum curcumin yield of 6.14 Box-Behnken Xu et al. (2015)
(Curcuma longa ([Bmim]Br), 1-hexyl-3-methylimidazolium based UAE; S: g/100g turmeric with large radical response surface
L.) bromide ([Hmim]Br), 1-octyl-3-methylimidazo­ Ionic liquids US: scavenging capacity was obtained design
lium bromide ([Omim]Br), 1-octyl-3-methylimida­ bath; PS:60–80 at ILs: [Omim]Br, IL
zoliumtetrafluoroborate ([Omim][BF4]); T: mesh; LSR: 30:1 concentration:0.42 mol/L; t: 90
25–65 ◦ C; P: 100–250 W; t: 10–90 min; IL min; & P: 250W.
concentration: 0.1–0.5 mol/L

flavonoid content of 1039.64 mg GAE (Gallic acid equivalent)/g and
492.57 QE (Quercetin equivalent)/g of ginger extract, respectively,
under optimum conditions. Besides, the ultrasound-assisted ginger
extract exhibited 54.5% of DPPH antioxidant activity and particularly
highest antimicrobial effect against Escherichia coli, Salmonella typhi­
murium, Bacillus cereus, and Staphylococcus aureus. Cebi et al. (2019) also
demonstrated that UAE maximized the cinnamon total phenolic content
(149.3 mg GAE/g DW) based on the fuzzy optimization, which repre­
sented the extraction time of 50 min at 70 ◦ C and ethanol concentration
of 72%. The UAE of cinnamon revealed the presence of trans-cinnamic
acid and p-coumaric acid with contents of 41 mg/g and 2 mg/g DW,
respectively. Furthermore, Aghajani et al. (2018) extracted the bioactive
and antioxidant compounds from Ferulago angulata by using the ultra­
sound bath, frequency of 40 kHz, exposure times (4, 6, and 8 min) and
elucidated that UAE intensified a total flavonoid content (0.56 mg RE
(Rutin equivalents)/g) in an extract under the ethanol concentration
(49.49% (v/v)) and extraction time (7.65 min), but the maximum DPPH
antioxidant activity (1.13 mg/g of extract) was obtained under 98.27%
(v/v) after 8 min. Tomšik et al. (2016) demonstrated that UAE maxi­
mized the extraction yield (38.1% (w/w)) of bioactive compounds from
wild garlic with higher total phenol (1.6 g GAE/100 g DW), total fla­
vonoids (0.35 g CE (Catechin equivalents)/100 g DW), and DPPH anti­
oxidant activity (0.71 mg/mL) under the extraction parameters of 70%
ethanol, 80 ◦ C, 79.8 min and 20.06 W/L ultrasonic power. Patil and
Rathod (2020) elucidated that ultrasound-assisted three-phase partition
extraction for 20 min showed the superior curcuminoids yield (67.15
mg/g DW) with a high total phenol content, antioxidant and
anti-inflammatory activity than the conventional three-phase partition
(58.38 mg/g DW) for 2.5 h.
Alexandru et al. (2013) carried out the pilot level UAE (batch and
continuous flow ultrasonic reactors) of phenolic compounds, using as
scaling parameter of 1 kg of clove and 20 L of ethanol as a solvent for the
fixed exposure time of 45 min. It resulted in a higher amount of total
phenolic compound with a best antioxidant activity and eugenol at
continuous flow cycles of 1350 mL/min and power density of 700 W/L.
This large-scale experiment elucidates that UAE can be an alternative for
bioactives extraction at the industrial scale level.
5.4. Other compounds
The other bioactive compounds include steroids, terpenoids, alka­
loids, carotenoids, pigments (Kumari et al., 2017). These compounds are
abundantly present in spices as secondary metabolites and UAE has been
employed to improve the extraction efficiency from the various spices
with short extraction time (Table 2(d)). Civan and Kumcuoglu (2019)
extracted the carotenoid and capsaicinoid from the pulp of hot pepper
paste and found that UAE with 60% amplitude at 60 ◦ C for 5 min in
probe-type induced the higher carotenoid content (230.54 mg β-car­
otene/100g DW), total capsaicinoid content (781.42 μg capsaicin/g
DW), total phenolic content (710.78 mg GAE/kg DW), and antioxidant
activity (189.25 μmol TEAC (Trolox equivalents antioxidant capacity)/g
DW) than those components obtained by maceration. Similarly, UAE
resulted in maximum piperine yield (5.8 mg/g) from the fruit of Piper
longum with a short extraction time (18 min) than the piperine yield
obtained by the Soxhlet extraction (1.67 mg/g) after 2 h and batch type
extraction (0.98 mg/g) after 8 h (Rathod & Rathod, 2014). Further, UAE
with a combination of aqueous (water and 50% ethanol) solutions as
solvent exhibited higher carotenoids from thyme and rosemary than the
conventional extraction under the same solvents (Munekata et al.,
2020). The amount of capsinoids (capsiate and dihydrocapsiate)

Table 2. (d)
Optimized conditions of ultrasound-assisted extraction (UAE) of other bioactives from spices.
Bioactives Spices Extraction variables Treatment Optimized conditions for UAE/ Optimization method References
Conditions Major findings

Alkaloids Piperaceae S: ethanol, Acetone, and US: bath; PS: Maximum yield of piperine of 5.8 NA Rathod and
(Piper longum) Hexane; t: 3–30 min; LSR: 0.4–0.55 mm mg/g was resulted at t:18 min, Rathod (2014)
2.5:1–40:1; DC: 20–100%; F: F:25 kHz, T:50 ◦ C, P: 125 W,
25 and 40 kHz; P: 100–200 W; DC:80%, LSR: 10:1 and S: ethanol
T: 30–70 ◦ C
Red Jalapeno T: 30–60 ◦ C; t: 5–20 min; P: US: probe; P: 400 The maximum amount of total Full factorial design Civan and
pepper 40–80% W; F: 24 kHz; DC: capsaicinoid content 1148 μg/g Kumcuoglu
(Capsicum 40%; S: olive oil; DM was obtained at P: 40%, T: (2019)
annuum L.) LSR: 0.4:1 40 ◦ C, and t: 15 min.
Dedo de moça P: 150, 300 & 450 W/cm2; T: US: probe; F:20 UAE with methanol reduced the Pseudo-first order, model based Dias et al.
pepper 40, 50 & 60 ◦ C; S: ethanol & kHz; P: 800 W capsaicinoid yields down to 50% on instantaneous washing by (2017)
(Capsicum methanol in comparison to the Soxhlet diffusion, & phenomenological
baccatum L.) extraction model
Carotenoid Red Jalapeno T: 30–60 ◦ C; t: 5–20 min; P: US: probe; P: 400 The maximum amount of total Full factorial design Civan and
pepper 40–80% W; F: 24 kHz; DC: carotenoid of 232.46 mg Kumcuoglu
(Capsicum 40%; S: olive oil; β-carotene/100 g DM was (2019)
annuum L.) LSR: 0.4:1 obtained at P: 60%, T: 60 ◦ C, and
t: 5 min.
Vitamins Black caraway P: 100, 200 & 300 W; t: 10, 15 US: probe; T: The maximum amount of Central composite response Shaterabadi
seeds (Carum & 20 min; type of sonication 40 ◦ C; F: 20 kHz; ascorbic acid and DPPH radical surface design et al. (2020)
carvi L.) (continuous, 4s on-2s off & 2s scavenging capacity was
on-2s off sonication) observed at P: 200 W, t:15 min,
and 4s on-2s off pulse sonication

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recovered from pepper fruits under optimum conditions of UAE was fluid extraction (Gavahian, Chu, et al., 2020; Wang et al., 2018; Wei
similar to that obtained by MAE (Vázquez-Espinosa et al., 2019). UAE et al., 2016).
recovered 90.7% of total capsaicin content from Habanero pepper,
which was abundantly higher than the soxhlet extraction (2.2%) and
6.1. Combination of supercritical fluid (CO2) and ultrasound extraction
shaking assisted extraction (76.1%) (Martins et al., 2017).
Vitamins are also a part of the bioactive compound, which possesses
Over the past few years, supercritical carbon dioxide (SC–CO2)
several biological activities. Shaterabadi et al. (2020) extracted the
extraction has been recognized as an alternative to traditional extraction
ascorbic acid from black caraway seeds and reported that UAE had a
methods because of the colorless, odorless, non-flammable, non-explo­
high extraction yield with stronger scavenging activity on DPPH radi­
sive, and non-toxic nature of carbon dioxide (CO2). In contrast, CO2 has
cals. However, limited investigations have been studied on the vitamins
a low dielectric constant, which resulted in a lower yield with less re­
and carotenoids extraction from spices by UAE. Overall, the enhanced
covery of targeted solute (Rawson et al., 2012). Thus, the co-solvents (i.
yields of alkaloids, carotenoids, and vitamins may be attributed to
e., methanol, ethanol and isopropanol) are included in order to increase
cavitation effects caused by UAE, which induce cell disintegration and
the polarity of the solvent during the extraction process (Lima et al.,
rapid inter-particle collisions fractures, and disruption in cell walls fa­
2019). The ultrasound-assisted supercritical carbon dioxide (USC–CO2)
cilitates the infiltration of extracting solvent into the cell tissue and
extraction triggers the solvent cavitation and micro-stirring during
diffusion of metabolites from plant matrix to the solvent (Khadhraoui
extraction process, which results in physical modifications, including
et al., 2018).
the cell wall rupture and increased solvent diffusion. These modification
causes faster mass transfer of targeted solute to the solvent, thereby
6. Integration of UAE with other emerging technologies
enhancing the extraction efficiency (Chemat et al., 2017; Dassoff & Li,
2019).
In a recent trend, there is a growing interest in green and environ­
Currently, USC-CO2 has been successfully investigated for the
ment friendly technologies, which can reduce the production cost,
extraction of various functional compounds from different plant prod­
shorten extraction time, enhance yield, accelerates extraction rate,
ucts but limited studies from spices (Said et al., 2015; Wei et al., 2016).
minimize energy usage and solvent with easier heat and mass transfer.
Said et al. (2015) reported USC-CO2 extraction of oleoresin from the
The combination of UAE with the other novel technologies (Microwave,
ginger rhizome by using methanol as co-solvent resulted in the
Enzyme, Ohmic heating, Pulsed electric field, and Supercritical fluid)
maximum yield (8.15%) at 35 ◦ C, pressure 25 MPa, after 1 h which was
would be the better option to get the balance between the product
significantly higher than the extraction yield obtained by SC-CO2
quality, production costs, and solvent consumption (Wen et al., 2020).
(6.87%) extraction at pressure 25 MPa, 40 ◦ C and CO2 flow rate of 15
Among them, UAE with combination of microwave and supercritical
g/min after 3 h, and soxhlet extraction (7.3%), 64 ◦ C after 6 h. Inter­
fluid assisted extraction is the commonly applied technology for the
estingly, Wei et al., (2016) extracted the α-humulene-enriched clove oil
extraction of various bioactives from spices, which are summarized in
by using the USC-CO2 extraction and elucidated that the USC-CO2
Table 3. Moreover, the integration of UAE with microwave and super­
method resulted in the higher yields of clove oil (23.31 g/g of clove) and
critical fluid treatments is mainly to overcome the limitations in
α-humulene (2.75 g/g of oil) under the optimized conditions, which
extraction process such as inhomogeneous heating in MAE, weak ther­
were superior to the yields obtained by SC-CO2 extraction (20.97 g/g of
mal effect in UAE, and high capital and operating costs in supercritical
clove; 1.89 g/g of oil), steam distillation (20.04 g/g of clove; 2.35 g/g of

Table 3
Applications of UAE in combination with other novel extraction technologies in bioactives extraction from spices.
Integrated novel spices Bioactives Treatment Conditions Major findings References
techniques

UAE coupled with White and black Essential oil PS: 40 mesh; LSR: 1:10; T: 100 ◦ C; ET: 7 min; P: Essential oil yield (4.1%) and superoxide Wang et al.
microwave-assisted peppers (Piper 50 W; microwave power: 500 W radical scavenging activity of white pepper (2018)
(MAE) nigrum L.) by UMAE were both significantly higher than
those oil extracted by MAE (3.7%) and UAE
(4.1%).
Black pepper Alkaloid PS:0.12–0.3 mm; S: ethanol, methanol, acetone, Maximum extraction yield of piperine was Gorgani
(Piper nigrum L.) and dichloromethane; LSR: 5:1–30:1; 46.6 mg piperine/g pepper which was et al. (2017)
Microwave power: 100 for 1min; T: 30–60 ◦ C; t: obtained at the PS: 0.15 mm, LSR: 20:1, S:
5–45 min ethanol, microwave power of 100 W for 1
min, and T: 50 ◦ C for t: 30 min, which was
greater than those resulted by Soxhlet (39.1
mg/g), MAE (38.8 mg/g) and UAE (37.0 mg/
g).
UAE coupled with Ginger (Zingiber oleoresin F: 40 kHz; P: 100 W; T: 60 ◦ C; t: 60 min; SC-CO2 Ultrasound-assisted SC-CO2 extraction was Said et al.
supercritical fluid officinale Roscoe) with pressure: 15–25 MPa & T: 30–40 ◦ C; CO2 found to be the best method of extraction (2015)
(SC–CO2) assisted flow rate: 10–20 g/min with the highest oleoresin yield of 8.15% at
extraction 35 ◦ C temperature and 25 MPa pressure than
(USC– CO2) the SC-CO2 assisted extraction yield of
6.87%.
Clove (Syzygium Essential oil T:32–50 ◦ C; pressures: 9–25 MPa; US: bath; PS: The yield obtained using USC–CO2 could be Wei et al.
aromaticum L.) and 0.355 mm; F: 40 kHz; P: 185 W; DC: 75%; CO2 significantly increased by 17% and the (2016)
α-humulene flow rate: 1.4 g/min; static extraction time of 15 extraction time decreased 45% as compared
min, and dynamic extraction time of 100 min to SC–CO2 extraction operating under T:
44 ◦ C and Pressure: 18.5 MPa.
Malagueta Alkaloid & P: 180, 280, & 360 W; t: 60, 180, & 240 min; US: USC- CO2 enhanced the oleoresin up to 30% Santos et al.
pepper (Capsicum oleoresin probe type; as compared with SC-CO2, without changing (2015)
frutescens L.) the total phenolic and capsaicinoids profile
in the extract at conditions of P: 360 W: 60
min, T: 40 ◦ C, pressure:15 MPa, & CO2 flow
rate of 1.673 × 10− 4 kg/s.

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oil), and heat-reflux extraction (17.20 g/g of clove; 1.71 g/g of oil)
methods.
6.2. Combination of microwave and ultrasound extraction
The combination of UAE and MAE has been successfully employed in
the form of simultaneous ultrasound-microwave assisted extraction
(UMAE), which is one of the most optimistic cost-effective hybrid
method because of its fast and efficient extractions (Chemat et al.,
2017).
The simultaneous UMAE is a complementary extraction method with
the supreme thermal effect of MAE which could effectively make up for
the problem of inadequate heat production by UAE, vice versa, the
mechanical oscillation and stirring action of UAE could effectively
compensate the uneven heat distribution by MAE (Wang et al., 2018).
However, UMAE has the limitation of lower power level (up to 90 W)
than the individual microwave and ultrasound energy source due to its
existence of nonmetallic ultrasound probes like quartz, Pyrex, PEEK
(polyether ether ketone), or PTFE (polytetrafluoroethylene), and that
intrinsic structure of nonmetallic probes could be irreversibly damaged
if maximum power level was more than 90 W (Wen et al., 2020).
Even though fewer studies reported the use of UMAE for spices,
Wang et al. (2018) have used UMAE treatment to white and black
peppers at 100 ◦ C, 500 W of microwave power, and 50 W ultrasound
power with 40 kHz of frequency for 7 min resulted in the high essential
oil yield (4.1%) and shorter extraction time (20 min) than individual
MAE (3.7% of oil yield after 30 min) and UAE alone (3.4% of oil yield
after 50 min). Furthermore, Gorgani et al. (2017) also stated that UMAE
resulted in maximum extraction yield (46.6 mg piperine/g of pepper)
from black pepper at the optimized conditions, which was significantly
higher than the yield obtained by soxhlet extraction (39.1 mg/g), MAE
alone (38.8 mg/g) and UAE alone (37.0 mg/g).
7. Optimization and mathematical modeling of UAE
methodology (RSM), which is a mathematical and statistical tool that
have been broadly applied to analyze and optimize the parameters. The
different RSM designs have been employed in optimizing the extraction
variables of the UAE process which is primarily dependent on selection
of independent factors (Table 4(a)). Among those RSM designs, central
composite design (CCD) and Box-Behnken design (BBD) are the most
commonly used and efficiently optimized methods. CCD has been used
for UAE of polyphenols from ginger (Murphy et al., 2020), phenolic
compounds from cinnamon (Cebi et al., 2019), antioxidant and bioac­
tive compounds from Ferulago angulata (Aghajani et al., 2018), essential
oil from clove (Tekin et al., 2015), ascorbic acid recovery from black
caraway seeds (Shaterabadi et al., 2020), cinnamic acid and cinna­
maldehyde from Cinnamomum cassia (Lee et al., 2018). While BBD used
for UAE of polysaccharides from fenugreek seed (Kia et al., 2018), and
Chrysanthemum morifolium cv. Hangju (Hou et al., 2020), capsinoids
from pepper fruits (Vázquez-Espinosa et al., 2019), curcuminoids com­
pounds from Curcuma longa L. rhizomes (Xu et al., 2015). Other than
these, central composite face-centered design and central composite
rotatable design for extraction of bioactive compounds from wild garlic
(Tomšik et al., 2016), and flavonoids and phenolic compounds from
Ocimum tenuiflorum leaves (Upadhyay et al., 2015) were used. The
regression analysis on the extraction results obtained from the applica­
tion of these RSM designs generates the polynomial equations.
Moreover, the other statistical techniques are also used in the UAE
process which includes the fuzzy logic model for phenolic compounds
extraction from cinnamon (Cebi et al., 2019), single-factor design for
flavonoids, and phenolic compounds extraction from Ocimum tenui­
florum leaves (Upadhyay et al., 2015) and polysaccharides extraction
from Chrysanthemum morifolium cv. Hangju (Hou et al., 2020), mixed
factorial 3⋅22 experimental design for Capsicum annuum oleoresin
extraction (Fernández-Ronco et al., 2013), the Taguchi methods of L16
orthogonal array for star anise oleoresin extraction (Li et al., 2018),
Cinnamomum cassia Bark Oil (Jadhav et al., 2020), and L9 orthogonal
array for Cinnamomum cassia Bark Oil (Chen, Sun, et al., 2020).

7.1. Optimization 7.2. Extraction kinetics

As reported in the above sections, all the parameters mentioned will
affect the extraction efficiency and yield of the UAE process. Although,
these parameters can interact together in the ultrasound system, and the
product of these parameters interaction will reflect on the biological
activity of spice extracts. The interactions of these extraction parameters
can be analyzed through the implementation of Response surface
The numerical optimization of process parameters in the UAE has
been extensively investigated by several researchers (Dias et al., 2017;
Dong et al., 2014; Santos et al., 2015; Wei et al., 2016; Yue et al., 2012).
Among them, Yue et al. (2012) described a mathematical model based
on Fick’s first law for explaining the extraction kinetics of capsaicin from
red peppers by using UAE and also demonstrated that this model was

Table 4. (a)
Applications of RSM models in UAE of bioactives from spices.
RSM models Spices Bioactives Regression equations: second-order polynomial model Process design References
equation

Box-Behnken Turmeric (Curcuma Phenolic compound- y1 = − 1.61816 + 36.38598x1 − 0.00855x2 + Three factor-five level design Xu et al.
response surface longa L.) Curcuminoids (y1 ) 0.00066x3 + 0.01368x1 x2 + 0.00576x1 x3 + (x1 = IL concentration; x2 = t; (2015)
design 0.0000366x2 x3 − 45.5718x21 − 0.0000275x22 − & x3 = P)
0.00000539x23
Fenugreek seed Polysaccharide (y1 ) y1 = + 33.31 + 0.50x1 + 1.07x2 + 0.96x3 + Three level-three factor design Das (2013)
(Trigonella foenum- 0.37x1 x2 − 1.18 x1 x3 − 0.73x2 x3 − 2.05x21 − (x1 = P; x2 = t; & x3 = LSR)
graecum) 3.18x22 − 2.39x23
Central composite Ginger (Zingiber Phenolic y1 = − 1439.76 + 8.51x1 + 56.803x2 + 22.407x3 + Five level-four factor design Murphy
response surface officinale) compounds: 1.193x4 − 0.107x12 − 0.087x1 x2 + 0.005 x1 x3 + (x1 = SC; x2 = t; & x3 = T; x4 = et al. (2020)
design polyphenols (y1 ) 0.008x1 x4 − 0.895x22 − 0.167x2 x3 − 0.015x2 x4 − LSR)
0.177x32 + 0.002x3 x4 − 0.0005 x42
Cinnamon Total Phenolic y1 = + 135.5 + 7.19x1 + 7.49x2 + 0.46x3 + Single level-three factor design Cebi et al.
(Cinnamomum compounds (y1 ) 3.33x1 x2 − 4.13 x1 x3 + 5.31x2 x3 − 12.83x21 − (x1 = ethanol concentration; (2019)
cassia) 2.85x22 + 1.76x23 x2 = T; & x3 = t)
Central composite Wild garlic (Allium Total Phenolic y1 = 1.2643 + 0.0314x3 + 0.0569x1 x2 + Three level-four factor design Tomšik et al.
face-centered ursinum L.) compounds (y1 ) & 0.1476 x1 x3 − 0.1072x1 x4 − 0.528x21 ; (x1 = T; x2 = ethanol (2016)
response surface Total flavonoid y2 = 0.13 + 0.1398x2 − 0.96x3 + 0.37x1 x2 − concentration; & x3 = t; x4 =
design content (y2 ), 1.18 x1 x3 − 0.73x2 x3 − 2.05x21 − 3.18x22 − 2.39x23 P)

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well fitted for optimizing the parameters. Dias et al. (2017) reported that
phenomenological model based on thermodynamics and mass transfer
well fitted for describing and optimizing the extraction kinetics of bio­
actives from Dedo de moca pepper by UAE. Further, Dong et al., (2014)
observed that the Two-site kinetic model has shown to be more suitable
in explaining the extraction kinetics of vanillin than the Elovich’s,
modified Peleg’s, and Power-law kinetic equations. The well-fitting of
the phenomenological model can attribute to the two-step kinetic
description process: bioactive extraction on or near the surface of the
solid matrix (washing process), followed by extraction of bioactives
located inside the cells of plant matrix (slow diffusion). Moreover,
Shirsath et al. (2017) have used a Peleg’s model for evaluating the
extraction kinetics of curcumin through varying UAE parameters and
optimized the extraction parameters to induce a maximum yield with
minimal time consumption by using the modified Peleg’s kinetic equa­
tion, represented in Table 4 (b).
The other kinetic models have also been broadly employed for pre­
dicting the extraction kinetics of bioactives from spices. Santos et al.
(2015) elucidated that the Sovova model based on broken and intact cell
concept was effective in predicting the extraction kinetics and mass
transfer coefficients of USC-CO2 of capsaicinoids from malagueta pep­
per. The density-based models such as Chrastil, Bartle, and Kumar, and
Johnston models were also found to fit the fictitious solubility of an
α-humulene compound in USC-CO2 extraction of essential from clove
(Wei et al., 2016). However, the second-order kinetic model was
adequate in describing the extraction kinetics of USC-CO2 of triterpenic
acids from Hedyotis diffusa and Hedyotis corymbosa tea by using the
activation energy in an Arrhenius equation as a function of extraction
rate and 1/absolute temperature (Wei & Yang, 2015). Overall, the
Two-site kinetic model and Peleg’s model are the most employed and
best fitted for describing the extraction kinetics of bioactives from spices
by UAE. The approach of these two models in optimizing the bioactive
extraction kinetics makes them a fundamental point of view in applying
the UAE process at the research and industrial level.
8. Effect of UAE process on the stability of bioactives from spices
UAE has proven to be a technology resulting in higher extraction
yield with a retention of essential compounds from spices. But, there is a
chance of potential degradation effect of UAE process on the stability of
bioactives during extraction which reflects on biological activity of spice
extracts and such stability largely relies on its chemical structure. For
example, longer exposure of ultrasound irradiation can cause the
degradation of polar bioactives and this degradation trend was observed
in the concentration of curcumin and curcuminoids by Binello et al.
(2020). The author quantified the degradation of curcumin and curcu­
minoids by HPLC (High-performance liquid chromatography) and 1H
NMR (Hydrogen/proton-Nuclear Magnetic Resonance). Similar degra­
dation in the phenolic compounds from ginger such as [6]-, [8]-,
[10]-gingerols and [6]-shogaol were also identified while increasing the
irradiation time from 5 to 30 min (Varakumar et al., 2017). The
degradation effects of the UAE process can be attributed to the pyrolysis
within the cavitation bubbles or nuclei; these are free-floating and very
small bubbles in the gas or liquid pockets trapped in the crevices of solid
boundaries in a liquid state, which is more likely to be the primer re­
action path for the degradation of polar bioactive. Secondly, the gen­
eration of hydroxyl radicals oxidizes the polar organic compounds such
as phenolic compounds, carotenoids, flavonoids, and ascorbic acid. The
radicals concentration is mainly frequency-dependent in linear mode,
but the traces of hydroxy and hydrogen radicals can form even at the low
frequencies (Kumari et al., 2017; Rawson, Tiwari, et al., 2011).
On the other side, the solvent type can also lead to different radical
concentration, which is critical for labile compounds stability. Like,
ultrasonication caused the milder radical formation in the presence of
ethanol than the ethyl acetate and these radicals facilitated the higher
degradation of curcumin and curcuminoids in ethanol rather than ethyl
acetate (Binello et al., 2020). Further, dichloromethane also caused the
degradation of all-trans-β-carotene contents extracted from mandarin
peel using UAE (Sun et al., 2011). Carail et al. (2015) also showed
similar degradation of all-E-β-carotene in the order of ultrasound time >
ultrasonic intensity > temperature. They identified that degradation was
more predominant in the aqueous system compared to organic solvents.
Among all bioactives, carotenoids are highly degraded because of their
poly-isoprenoid structure conferring a long chain of conjugated double
bonds which makes them chemically sensitive (Saini & Keum, 2018).
Therefore, these studies are evident that the vast majority of

Table 4. (b)
Applications of kinetic models in UAE of bioactives from spices.
Bioactives Spices Kinetic equations Kinetic Models Key findings References

α-humulene Clove (Syzygium ln(y2 ) = a0 + Chrastil’s density model Chrastil, Bartle, and Kumar & Johnston mathematical Wei et al.
enriched aromaticum L.) a2 Kumar and Johnston models were found to fit the fictitious solubility of (2016)
a1 ln(ρ) +
essential oil T Bartle α-humulene in USC- CO2 assisted extracted clove oil very
ln(y2 ) = b0 + b1 ρ + well.
b2
T( )
y2 P
ln = A+
Pref
c1 (ρ − ρref )
Phenolic Vanilla pods Ceq t Modified Peleg’s Two site kinetic model had the lowest RMSD and resulted in Dong et al.
Ct =
compound- (Vanilla planifolia k+t Elovich’s better agreement between the experimental and theoretical (2014)
vanillin Andrews) Ct = E ln(t) + a Power-law data in the extraction kinetics of vanillin than the other
Ct = Btn Two Site kinetic models.
Ct = Ceq [1 −
f exp( − k1 t) − (1 −
f) exp( − k2 t)]
Bioactive Dedo de moca y = y∞ [1 − f exp( − Phenomenological model Phenomenological model provided a good fit of the Dias et al.
compounds pepper (Capsicum k1 t) − (1 − f) (Two site kinetic model) extraction kinetics in all experimental conditions and (2017)
baccatum L.) exp( − k2 t)] Pseudo-first order model elucidated that ultrasound influences both washing and
y = y∞ [1 − exp( − Model based on slow diffusion steps.
k2 t)] instantaneous washing
y = y∞ [1 − (1 − f) followed by diffusion
exp( − k2 t)]
Phenolic Mango ginger Ceq t Modified Peleg’s model Peleg’s model was satisfactorily described the extraction Shirsath
Ct =
compound- (Curcuma amada) k1 + k2 t kinetics of curcumin with reasonable accuracy. et al. (2017)
Curcumin

988
M.V. Rao et al.
investigations have primarily focused on the quantity of the compound
rather than the structure and a kind of new compounds formed by the
degradation process.
9. Gap and future trends for research and industrial-scale
processing
The energy and environmental assessment of the UAE process is
needed in the future to compare with the novel and conventional
extraction methods when used for bioactives extraction from spices. The
use of UAE in combination with the other emerging extraction tech­
nologies such as MAE, ohmic assisted extraction, enzyme assisted
extraction, SC-CO2, and pulsed electric field for the extraction of
bioactive components from spices is limited and needs to be further
explored. The technological variations in the use of these combined
technologies to spices as a sequential extraction and simultaneous/
coupled extraction needs to be investigated. The studies on the stability
of individual extracted bioactive compounds during UAE from spices
provide a unique approach for further research. The development of
ultrasonic equipment with a feature of multiple frequencies exposed to
the extraction medium without making a direct contact to ultrasonic
horns would improve the commercial visualization of the UAE of
bioactive components from spices. Moreover, the application of UAE
technology to the food industry requires a high amount of energy and
hence optimization of scalable parameters on the bulk quantity of spices
is required. Therefore, the research of UAE process on the industrial
scale should be strengthened in terms of high power process design, easy
installation, and low maintenance costs.
10. Conclusion
UAE creates physical modification to the inherent matrix of spices
which fast-tracks the extraction of targeted components. Further it re­
duces extraction time, energy, solvent requirement and hence toxic
residue production. Ultrasonic cavitation intensifies the extraction yield
of heat labile essential oils and phenolic compounds from spices. It en­
hances oleoresin yield at lower temperature compared to conventional
extraction methods that would have resulted in unacceptable yield
under similar conditions. Combination of UAE with other technologies
would create a balance between the product quality, production costs,
and solvent consumption. Two-site kinetic model and Peleg’s model are
the best fitted for studying the UAE kinetics of bioactives from spices.
The clean and green technology aspect of ultrasound treatment is the
need of hour. And have shown promising results even in extraction of
bioactives from spice wastes. Few limitations which still need to be
addressed are industrial-scale bulk treatment plant where the uniformity
of energy flux for a continuous treatment is dependent on its design
criteria which requires further research and improvement.
Author contributions
All authors contributed equally for the manuscript, to critically re­
view all previous research, draft the manuscript and to prepare the ta­
bles and figures.
Declaration of competing interest
The authors declare no conflict of interest.
Acknowledgement
We would like to thank Ministry of Food Processing Industries,
Government of India for funding our work (Q-11/10/2021-R&D).
989
Trends in Food Science & Technology 116 (2021) 975–991
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