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A comparative study of various oil extraction

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Article in Reviews in Chemical Engineering · December 2014

DOI: 10.1515/revce-2013-0038

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 Rev Chem Eng 2014; 30(6): 605–626

Jibrin Mohammed Danlami, Agus Arsad*, Muhammad Abbas Ahmad Zaini

and Hanizam Sulaiman

A comparative study of various oil extraction

techniques from plants
Abstract: Researchers have shown that techniques such 1 Introduction
as microwave-assisted extraction, ultrasound-assisted
extraction, pressurized liquid extraction, and supercriti-
Extraction is an important step for the separation, iden-
cal fluid extraction developed for extraction of valuable
tification, and use of valuable compounds from different
components from plants and seed materials have been
plants (Stevigny et al. 2007). The choice of an acceptable
successfully used to effectively reduce the major short-
technique to obtain maximum yield and highest purity
comings of the traditional method such as Soxhlet extrac-
varies according to the nature of the target compound.
tion. These include shorter extraction time, increase in
Numerous chemical and mechanical processes like
yield of extracted components, decrease in solvent con-
solvent extraction and steam distillation are used for the
sumption, and improvement of the quality of extracts.
extraction of compounds from plants (Shirsath et al. 2012).
This review presents a detailed description of the princi-
The existing techniques used for the extraction of essen-
ples and mechanisms of the various extraction techniques
tial oils, fat, and oils include Soxhlet, hydrodistillation,
for better understanding and summarizes the potential of
and maceration with alcohol (Wang and Weller 2006). The
these techniques in the extraction of oil from plants and
mass transfer resistances due to the involvement of more
seed materials. Discussions on some of the parameters
than one phase within the system repeatedly limit the use
affecting the extraction efficiency are also highlighted,
of traditional Soxhlet extraction techniques (Jadhav et al.
with special emphasis on supercritical fluid extraction.
2009). This separation method requires a very long time
A comparison of the performance of traditional Soxhlet
depending on the diffusion rates of solvents. Furthermore,
extraction with that of other extraction techniques is also
standard extraction techniques are energy intensive (Puri
presented.
et al. 2012). These techniques are manual processes, and
reproducibility is a major challenge (Shen and Shao 2005).
Keywords: microwave assisted extraction; pressur-
Thermally sensitive components are deteriorated by the
ized liquid extraction techniques; Soxhlet extraction;
heating process, resulting in low extraction yields. These
supercritical fluid extraction; ultrasonication assisted
active molecules might be altered by the pH, temperature,
extraction.
and pressure conditions used. The limitations mentioned
above, combined with the significant increase in the
DOI 10.1515/revce-2013-0038 demand for bioactive components, essential oils, fat, and
Received November 18, 2013; accepted July 30, 2014; previously oils, have prompted the need for appropriate, selective,
published online September 4, 2014
cost-saving, and eco-friendly extraction technologies that
are rapid, produce higher yields, and comply with relevant
legislation (Ibáñez et al. 2012). This has led to the develop-
ment of novel extraction processes, such as supercritical
fluid extraction (SFE), to enhance the product quality and
*Corresponding author: Agus Arsad, Enhanced Polymer Research
the quantity of the active natural products (Sajfrtová et al.
Group (ENPRO), Faculty of Chemical Engineering, Department of
Polymer Engineering, Universiti Teknologi Malaysia, 81310 UTM 2010, Bimakr et al. 2012).
Johor Bahru, Malaysia, e-mail: agus@cheme.utm.my In the last few years, SFE has received significant
Jibrin Mohammed Danlami and Muhammad Abbas Ahmad Zaini: attention as a promising alternative to conventional tech-
Centre of Lipid Engineering and Applied Research (CLEAR), Faculty nology for separation of various valuable compounds from
of Chemical Engineering, Universiti Teknologi Malaysia, 81310 UTM
natural sources (Gomes et al. 2007, Liu et al. 2010). This is
Johor Bahru, Malaysia
Hanizam Sulaiman: Centre for Information and Communication
because the technique is generally performed at low tem-
Technology (CICT), Universiti Teknologi Malaysia, 81310 UTM Johor peratures and short extraction times and a little amount
Bahru, Malaysia of solvent is used as compared with traditional extraction

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606      J.M. Danlami et al.: A comparative study of extraction
methods (Liza et  al. 2010). Supercritical carbon dioxide
(SC-CO2) extraction has attracted a lot of interest because
carbon dioxide (CO2) is an inert, low-cost, nontoxic, and
environmentally-friendly solvent that permits extraction
at low temperatures and comparatively low pressures.
In addition, CO2 can evaporate instantly when exposed
to atmospheric conditions (Herrero et  al. 2010). As CO2
is a nonpolar solvent, adding a little quantity of polar
solvents as cosolvent can greatly enhance the extraction
efficiency of polar compounds. Among the prominently
used solvents, ethanol (EtOH) is the most commonly used
because of its high miscibility with CO2, nontoxicity, and
allowed use in the food and pharmaceutical industries
(Herrero et al. 2010). SC-CO2 has been found to be selective
in the isolation of desired compounds without leaving any
toxic residues in the extracts and with no risk of thermal
degradation of the processed product. In reality, SC-CO2
extracts are most often recognized as safe to use in food
products (Gerard and May 2002). Extraction with SC-CO2
has become comparatively mature with potential applica-
tions for the extraction of valuable compounds from solid
plant matrices and seed oil.
Numerous review articles have been published on
Soxhlet extraction (Luque de Castro and Priego 2010),
microwave-assisted extraction (MAE) (Kaufmann and
Christen 2002, Tripti et  al. 2009), ultrasound-assisted
extraction (UAE) (Vinatoru 2001, Patist and Bates 2008,
Vilkhu et  al. 2008), pressurized liquid extraction (PLE)
(Kaufmann and Christen 2002, Smith 2002), and SFE
of vegetable materials (Sovová and Stateva 2011). The
present review focuses on issues arising from the appli-
cations of several extraction techniques such as Soxhlet
extraction, MAE, UAE, PLE, and SFE. The principle and
mechanisms of each extraction technique and factors
affecting SFE, such as temperature and pressure, effects
of modifier, extraction mode, and extraction time, are
discussed. Finally, potential applications and demerits of
these extraction methods are also reviewed.
2 Extraction techniques
2.1 Traditional Soxhlet extraction
2.1.1 Principles of operation
Basic techniques for the extraction of fat and oils
from seed matrices are based primarily on the selec-
tion of solvent, including the use of heat and agitation.
Soxhlet extraction, which has been the oldest method of
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extraction, is the most referenced technique for evalu-
ating the performance of other solid-liquid extraction
methods except in restricted fields of applications, such
as the extraction of thermolabile compounds (Luque de
Castro and Priego 2010). An overview of Soxhlet extrac-
tion of solid materials has been reported by Luque de
Castro and Priego (2010).
Figure 1 shows the standard Soxhlet system. The seed
materials (solids) are placed in the thimble-holder and
filled with condensed fresh solvent from a distillation
flask. As the liquid reaches an overflow level, a siphon
aspirates the solution of the thimble-holder and unloads
it into the distillation flask, carrying extracted solutes into
bulk of the liquid. In the solvent flask, solutes are sepa-
rated from the solvent using distillation. Solutes are left
in the flask and fresh solvent passes into the solid bed.
The operation is repeated until complete extraction is
achieved.
Soxhlet extraction and heat reflux extraction are not
the same process. Heat reflux extraction can be performed
simply by boiling the material in the solvent, where a
chilled surface is used to condense the rising solvent
vapors as they boil off and return them to a liquid state in
the container, without boiling away. The extract contin-
ues to concentrate in the solvent and is reduced to essence
later. Soxhlet extraction, on the other hand, is for separat-
ing parts that are soluble in a solvent.
Condenser
Extractor
Siphon
Sample
Distillation
flask
Heat source
Figure 1 Soxhlet extractor.

2.1.2 Solvent selection
An appropriate extracting solvent ought to be selected for
the extraction of targeted component using the Soxhlet
extraction technique. Different solvents will yield entirely
different extracts and extract compositions (Zarnowski
and Suzuki 2004). The most generally used solvent for
extraction of edible oils from plant sources is hexane.
This is due to its low boiling temperature and easy recov-
ery and since most oils are soluble in hexane. The disad-
vantage of n-hexane is its hazardous air pollution level
(Mamidipally and Liu 2004). The use of alternative sol-
vents such as isopropanol, ethanol, hydrocarbons, and
water has increased because of environmental, health,
and safety considerations. d-Limonene and hexane
have been employed in the extraction of oil from rice
bran (Mamidipally and Liu 2004). It was observed that
d-limonene extracted a considerably higher quantity of oil
than hexane did under any given set of conditions. At a pH
of 12, water (H2O) was used to extract rice bran oil (Han-
moungjai et al. 2000). The oil extracted using the aqueous
medium had a lower content of free fatty acid (FFA) and
color imparting than did oil extracted using hexane. Low
FFA offers low initiation of products’ oxidation and color-
ing of materials. However, using different solvents often
results in less recovery because of a decrease in molecular
affinity between solvent and solute. The costs of alterna-
tive solvents such as acetone and ethanol (hexane is the
standard) may be higher. A cosolvent is commonly added
in order to increase the polarity of the liquid phase. A
mixture of solvents such as isopropanol and hexane has
been reported to increase the yield and kinetics of the
extraction (Li et al. 2004).
2.1.3 B
 enefits and drawbacks of Soxhlet extraction
techniques
The benefits of conventional Soxhlet extraction method
include (a) keeping the system far from equilibrium by
constantly exposing the solid matrix to fresh solvent, (b)
maintaining high extraction temperature to enable recov-
ery of the compounds of interest, and (c) not requiring fil-
tration after leaching. Additionally, the Soxhlet extraction
is a very simple and a low-cost technique (Luque de Castro
and Priego 2010).
The major disadvantages of conventional Soxhlet
extraction method include the following: (a) the extrac-
tion time is lengthy and the process is labor intensive; (b) a
considerable amount of solvent is consumed; (c) agitation
cannot be provided in the extraction device to speed up
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J.M. Danlami et al.: A comparative study of extraction      607
the process; (d) the large solvent used needs an evapora-
tion/concentration procedure; (e) there is risk of thermal
decomposition of the target compounds; (f) there is no
selective extraction; and (g) the process allows manipula-
tions of limited variables. The time and the requirement
of a large amount of solvent result in wide criticism of
Soxhlet extraction technique (Luque de Castro and Priego
2010).
2.2 MAE
A microwave is referred to as a nonionizing electromag-
netic radiation that has a frequency of 300 MHz–300 GHz.
MAE transfers energy to the heated solvent such as metha-
nol or methanol/water mixture for polar compounds and
hexane for nonpolar compounds by twin mechanisms of
dipole rotation and ionic conduction. The target for micro-
wave heating, in most cases, is dried plant materials;
however, the plant cells still contain traces of moisture.
The moisture, when heated up within the plant cell due to
microwave effect, evaporates and generates high pressure
on the cell wall and results in swelling of the plant cell
(Vivekananda et al. 2007). This pushes, stretches, and con-
sequently ruptures the cell wall. These facilitate leaching
of active constituents from the cells to the solvent, thereby
enhancing the yield of oil. This phenomenon could be
intensified as the solvent is impregnated into the plant
matrix at a high heating efficiency of the microwave. The
bonds of cellulose (the main constituent of plant cell wall)
break down (hydrolyzed) at high temperature attained by
microwave radiation and are converted into soluble frac-
tions in 1–2 min. The attainment of higher temperature
by the cell wall during MAE leads to the dehydration of
cellulose and thereby reduces its mechanical strength
and also enhances solvent movement to the compounds
inside the cell (Latha 2000). A study of cell damage in
MAE experiments on tobacco leaf was conducted by scan-
ning electron microscopy (Zhou and Liu 2006). Scanning
of the untreated sample, MAE sample, and a sample from
heat-reflux extraction revealed no structural distinction
between heat-reflux extraction and the untreated samples,
except slight ruptures of the sample surface. However, the
sample surface was greatly destroyed after MAE. This sug-
gests that microwave treatment affected the structure of
the cell as a result of the sudden rise in temperature and
internal pressure increase.
During the process, exudation of the chemical sub-
stance occurring in the cell to the surrounding solvents
takes place. This mechanism of exposing the sample to the
solvent is not different from that of heat-reflux extraction
608      J.M. Danlami et al.: A comparative study of extraction
that solidly depends on permeation and solubilization
processes of bringing the analytes out of the matrix. A
destructive change in orange peel as a result of micro-
wave treatment was also observed using scanning elec-
tron micrographs (Kratchanova et al. 2004). The changes
in plant tissue because of microwave heating gave an
increased yield of extractable pectin. Furthermore, the
movement of dissolved ions increased solvent penetra-
tion into the matrix, thereby facilitating the release of
chemicals. It was also observed during the extraction of
essential oils from plant sources that MAE permits the
desorption of compounds of interest out of the plant. This
is a result of the targeted heating of the free water mol-
ecules in the gland and vascular systems, which leads to
localized heating leading to enlargement and subsequent
rupture of their walls, thereby allowing oil to flow toward
the organic solvent (Garcia-Ayusa et al. 2000, Kubrakova
and Toropchenova 2008). In fact, microwave energy is
dependent on the dielectric susceptibility of the solvent
and plant matrix. Most of the time, the sample is immersed
in a solvent that absorbs microwave energy strongly. An
increase in the solvent temperature allows its penetra-
tion into the sample and the constituents are released
into the hot solvent (Routray and Orsat 2012). However,
in some cases, only selective heating of the sample matrix
is brought about by immersing the sample in a micro-
wave transparent solvent (hexane and chloroform). This
approach is useful for thermolabile compounds to prevent
their degradation (Vivekananda et al. 2007).
There are two types of MAE systems, the closed vessel
and the open vessel. Closed vessels are for the extraction
of target compounds at high temperature and pressure
conditions, while open-vessel systems are for extractions
carried out at atmospheric pressure conditions (Kaufmann
and Christen 2002). MAE extraction technology has been
applied for both laboratory-scale level and large-scale
industrial operations, that is, full-scale commercialized
extraction applications (Ying et al. 2013). During the last
few years, the MAE technology has been used for isolating
essential oils, fats, and oils (Deng et  al. 2006, Bayramo-
glu et al. 2008). Microwave technology has been found to
be a rapid, safe, and low-cost technique for the extraction
of essential oils, fats, and oils and does not need samples
devoid of water (Chemat et al. 2006, Bousbia et al. 2009).
In an attempt to improve Soxhlet performance, the most
successful has been the use of microwaves, which has pro-
vided a wider variety of approaches. In fact, microwave-
assisted Soxhlet extraction remains the most interesting
improvement of conventional Soxhlet extraction (Li et al.
2006). Microwave-assisted Soxhlet extraction of solids of
low-polar and nonpolar extractants comprises heating
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these up to their boiling point by using microwaves while
stirring with a magnetic stirrer to absorb microwave
radiation. Therefore, unlike classical conductive heating
methods, microwave heats the whole sample simultane-
ously. In this way, solvent vapors penetrate through the
sample and are condensed on arrival at the condenser, as
shown in Figure 2. With water running through the con-
densation pipe of the MAE system, the sample is mixed
with the extraction solvent, and the suspension is irradi-
ated with microwaves in a presetting procedure to reach
the desired temperature. The microwave irradiation power
is set as required until a complete extraction is achieved.
Results from numerous biological samples obtained by
this technique are qualitatively and quantitatively com-
parable with the steam distillation (Ferhat et  al. 2006,
Bendahou et al. 2008, Sahraoui et al. 2008, Farhat et al.
2009, 2011). However, it still uses organic solvents, such
as hexane, and therefore cannot be considered as a green
technology.
2.2.1 Solvent choice and volume
A major factor that affects extraction is the selection of
the appropriate solvent. The choice of solvent is based
mostly upon the solubility of the required analyte, the
ability of the solvent to interact with the matrix, and its
absorbance of microwaves (Chen et al. 2008). The solvent
selected should have a high selectivity of the analyte of
interest over the matrix components and should be com-
patible with further chromatographic analytical steps.
Transparent solvents are not heated under the microwave,
and those with high absorbing capability get heated
faster to enhance the extraction. Hexane is referred to be
To drain
Energy attenuator
Condensation pipe
Connecting tube Cooling water
Shield Temperature
250 ml boiling flask
thermistor recorder
Time presetting
Microwave cavity
Time controller
Magnetic stirrer
Figure 2 Schematic diagram of microwave-assisted Soxhlet
extractor.

a transparent solvent of the microwave, while ethanol is
regarded as an excellent microwave absorbing solvent.
Researchers have used solvent mixtures of high and low
microwave absorbability to get the optimum extraction
yields. There should be sufficient solvent to immerse
the plant matrix throughout the irradiation process. In
conventional extraction, higher solvent volume to solid
matrix gives higher extraction yields, whereas in MAE,
higher solvent might not give higher yield because of non-
uniformity and exposure to microwaves.
2.2.2 Benefits and drawbacks of MAE
MAE is a viable possibility for the extraction of essential
oils, fats, and oils from seeds due to its distinct benefits
over solvent extraction techniques (Cintas et  al. 2013).
MAE is comparable with other alternative modern extrac-
tion techniques due to its simplicity and low cost of equip-
ment. Other benefits of this extraction technique include
the following: (a) reduced extraction time; (b) allowing
of simple, rapid, and low solvent usage; (c) ability to add
re­agents during treatment; (d) extraction reaction controlled
by temperature and pressure control; (e) in processing
applications, ability to instantaneously shut the heat
source, which makes enormous difference to the product
quality and, hence, production economics; (f) higher
volume of raw material is processed over a given period;
(g) safe, with no potential hazard; (h) selective heating of
the sample solvent mixture; and (i) use of the technology
for chemical reaction such as hydrolysis. However, com-
pared with other modern extraction techniques, an addi-
tional stage (filtration or centrifugation) is required for
the removal of solid residues (Shah and Rohit 2013). Fur-
thermore, the efficiency of microwaves can be very poor
when either the target compounds are nonpolar or they
are volatile. In addition, MAE is not suitable for use when
considering heat-sensitive compounds because they will
be denatured. The analyte recovery is low, high pressure
usage may lead to explosion, and large cooling or venting
times are needed after the extraction process.
2.3 UAE
Ultrasound waves are regarded as high-frequency sound
waves above human hearing, that is, above 20 kHz. These
waves are propagated by rarefactions and compression.
This expansion causes negative pressure in the liquid.
If the pressure exceeds the tensile strength of the liquid,
formation of vapor bubbles occurs. These vapor bubbles
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J.M. Danlami et al.: A comparative study of extraction      609
go through implosive collapse in ultrasound fields, which
is called cavitation (Luque-García and Luque de Castro
2003). The implosion of cavitation bubbles generates
macroturbulence, at higher-velocity interparticle colli-
sions, and perturbation in microporous particles of the
biomass (Shirsath et  al. 2012). Cavitation close to the
liquid-solid interfaces directs a fast-moving stream of the
liquid through the cavity at the surface. Impingement by
these microjets leads to surface peeling, erosion, and par-
ticle breakdown, facilitating the release of bioactives or
the targeted compound from the biological matrix. This
results in an increase in the efficiency of extraction by
increasing mass transfer by eddy and internal diffusion
mechanisms (Vilkhu et  al. 2011). The mechanical effects
of ultrasound enable a larger penetration into cellular
materials and thereby improve mass transfer. Ultrasound
disrupts biological cell walls to facilitate the release of
contents. Therefore, cell disruption and effective mass
transfer are cited as major factors enhancing extraction
with ultrasonic power. Ultrasound permits changes in pro-
cessing conditions like a decrease in pressure and temper-
ature from those utilized in other extraction techniques,
allowing the extraction of thermolabile compounds
(Shah and Rohit 2013). For solid-hexane extraction of
pyrethrines from pyrethrum flowers without ultrasound,
extraction yield increases with extraction temperature,
and maximum yield is achieved at 339K. With ultrasound,
the effect of temperature on the yield is negligible in the
range of 313–333K, so that optimal extraction occurs at the
temperature range of 313–333K. Therefore, the use of UAE
is advisable for two compounds, which may be altered
under Soxhlet and heat reflux extraction operating condi-
tions due to high extraction temperature (Romdhane and
Gourdon 2002).
There are two types of ultrasound equipment that may
be used for extraction purposes, an ultrasonic water bath
and an ultrasonic probe system fitted to horn transducers
(Ibáñez et  al. 2012). Figure 3 shows a UAE system using
an ultrasonic probe. UAE extraction technology has been
used from laboratory-scale level to larger-scale indus-
trial operations, for commercialized extraction applica-
tions (Vilkhu et  al. 2008, Chemat et  al. 2011). UAE has
been widely used for the extraction of nutritional mate-
rial, like lipids (Metherel et al. 2009), proteins (Zhu et al.
2009), flavoring (Chen et  al. 2007, Da Porto et  al. 2009),
essential oils, fats, and oils (Kimbaris et  al. 2006), and
bioactive compounds (e.g., flavonoids) (Ma et  al. 2008),
carotenoids (Sun et al. 2006, Yue et al. 2006), and polysac-
charides (Iida et al. 2008, Chen et al. 2010, Wei et al. 2010,
Yan et al. 2011). UAE was also reported for the extraction
of oil from rapeseed (Ibiari et  al. 2010) and Monopterus
610      J.M. Danlami et al.: A comparative study of extraction
Transducer
Ultrasonic probe
Ultrasound
generator
h-depth of probe
in liquid
Jacketed glass beaker
Figure 3 Schematic diagram of UAE (adapted from Shekhar et al.
2013, reproduced with permission from the American Chemical
Society).
albus (Abdullah et al. 2010). Studies regarding the impact
of various solvents and their mixture, impact of solvent
volume, sonication time, and power indicated that UAE
has the potential to enhance extraction efficiency and to
also reduce the processing time, and the oil composition
was not denatured by the use of ultrasound.
2.3.1 Benefits and drawbacks of UAE technique
UAE is a simple, cost-effective, and efficient alternative
compared with traditional extraction techniques. The
benefits of using ultrasound in solid-liquid extraction are
to increase the extraction yield and fasten the kinetics.
Ultrasound facilitates the extraction of thermally sensi-
tive compounds. The costs of equipment are lower than
those of other new alternative extraction techniques. It
could be used with a wider variety of solvents, including
the aqueous extraction, for water-soluble components
and other solvents like ethanol and methanol (Chemat
et  al. 2011). Compared with Soxhlet extraction methods,
ultrasound extraction can enhance extraction efficiency
and extraction rate, reduce extraction temperature, and
increase the choice ranges of solvents (Vilkhu et al. 2008).
For example, the ultrasound was found to have no effect
on the composition of almond oil; however, the ultrasonic
cavitating energy can cause structural breakage of the
almond powder and greatly reduce the extraction time
(Zhang et al. 2009). In view of its growing use for isolat-
ing or separating organic compounds and its advantages,
the future introduction and dissemination of ultrasound
equipment appear to be assured for rapid essential oil
extraction. The shortcomings include wave attenuation
in the dispersed phase and a decrease in the sound wave
amplitude with distance, which is a major challenge in
UAE technologies. In fact, the activated ultrasound zone
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is restricted to a limited zone in the vicinity of the ultra-
sound emitter. These factors must be carefully considered
in the design of UAE.
2.4 PLE techniques
PLE is known also as accelerated solvent extraction, pres-
sure fluid extraction, high-pressure solvent extraction,
and enhanced solvent extraction (Nieto et al. 2010). The
temperature and pressure conditions utilized in PLE are
within the ranges of 323–473K and 3.5–20 MPa, respec-
tively. The elevated pressure causes the solvent tempera-
ture to rise above the normal boiling point temperature.
The increase in temperature tends to accelerate the extrac-
tion rate by increasing solubility and mass transfer rate.
Also, the increased temperature reduces the viscosity and
surface tension of solvents, helping them to spread evenly
over the biological matrix and improve the extraction rate.
In some cases, pressurized hot water is employed as a
solvent for extraction rather than an organic solvent. This
method is called pressurized hot water extraction or sub-
critical water extraction (Eskilsson et al. 2004).
A schematic diagram of a PLE system is shown in
Figure 4. The PLE equipment involves an extraction cell
where the sample is introduced. The cell is filled with a
solvent that is heated. High temperature and pressure are
then maintained to facilitate faster extraction. The equip-
ment has a pressure relief valve that guards against over
pressurization of the cell. Nitrogen is used to purge all the
residual solvents at the end of the extraction (Kaufmann
and Christen 2002). Extraction solvent, temperature, pres-
sure, numbers of cycles, and time are reported to influ-
ence extraction yield and rate (Nieto et al. 2010).
Purge Pressure
relief valve
valve
Oven
Pump Extraction
cell
A B C
Solvents
Nitrogen
Collection vessel
Waste vial
Figure 4 Schematic diagram of PLE (adapted from Shekhar et al.
2013, reproduced with permission from the American Chemical
Society).

Oilseeds like canola, corn, flax, cotton, soybeans, etc.,
have been reported to be extracted in no time, with higher
yield and improved quality through PLE compared with
the traditional methods, such as Soxhlet extraction. David
and Bruce (2010) examined the influence of elevated tem-
peratures on the oil during the extraction by PLE. It was
found that peroxide values were <5 ppm, which shows
no oxidation compared with Soxhlet. The FFA data also
showed no significant oxidation degradation occurred
during PLE.
2.4.1 Solvent choice
An ideal solvent for the extraction of oil from seed mate-
rials includes a high partition coefficient and high selec-
tivity with regard to the compound of interest, a large
extraction capacity, absence of irreversible reactions
between the solvent and oil, and ease of oil recovery
(Gertenbach 2002). The major factors to be considered
for optimal extraction are the mass transfer mechanisms,
characteristics of the seeds, and cost of the solvents
(Waldeback 2005).
2.4.2 Benefits and drawbacks of PLE techniques
The benefits of PLE include the following: (a) better extrac-
tion kinetics is achieved because of increased operating
temperature; (b) operating parameters can be changed to
increase selectivity; (c) accuracy and reproducibility are
better compared with conventional methods; (d) inert
nitrogen reduces the oxidation risk compared with con-
ventional extraction processes; (e) application method
is relatively simple; (f) there is lesser extraction time and
reduced solvent consumption; and (g) automation is pos-
sible and is easier compared with other extraction tech-
niques. The method also uses nontoxic extracting solvents
like CO2 and water, which has economical and environ-
mental benefits (Mustafa and Turner 2011). PLE is consid-
ered as a possible alternative for the extraction of polar
compounds (Brachet et al. 2001).
The drawbacks include the following: (a) extraction is
performed at high temperature; consequently, it will lead
to thermal degradation, especially for thermolabile com-
pounds in the extracts; (b) selectivity is achieved only by
varying the solvent type, which tends to be exhaustive and
may thus lead to nonselective extractions (Ibáñez et  al.
2012); (c) postextraction cleanup is necessary; and (d)
nowadays, it is used only for analytical purposes because
it has not yet been up-scaled.
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J.M. Danlami et al.: A comparative study of extraction      611
2.5 SFE
2.5.1 Process description, equipment, and cost
Supercritical fluid technology is recognized as an effec-
tive technique that has been used for laboratory-scale
level, to preparative scale, to pilot scale, and up to
larger-scale industrial commercial production, with high
efficiency comparable with that of existing chemical
analysis procedures (Sahena et  al. 2009). It is possible
to obtain more information on the extraction processes
and mechanisms using SFE, which is useful in the quan-
titative evaluation of the extraction efficiency and appro-
priate optimization of the process (Lang and Wai 2001).
The extracting solvent in this process is a fluid (dense
gas) at a temperature and pressure above the critical
values, TC and PC. SFE is applicable for the qualitative
and quantitative identification of constituents of natural
products, including heat-labile compounds (Mohamed
and Mansoori 2002). In SFE, several factors like tempera-
ture, pressure, sample volume, cosolvent addition, and
flow and pressure control play a vital role during extrac-
tion by SFE (Higuera-Ciapara et al. 2005). In conditions
that are fairly higher than the critical temperature and
pressure, supercritical fluids exhibit properties inter-
mediate to those of the liquid and gaseous phases. This
fluid possesses properties bounded by the extremes of
the gaseous and liquid states, and these properties could
be adjusted with alteration of the applied pressure and
temperature (Kroon and Raynie 2010). At suitable con-
ditions, any fluid can reach its supercritical state. The
chances of using supercritical fluids as extracting sol-
vents are directly linked to their density. The reduced
temperature Tr (i.e., T/TC) of supercritical fluid must not
exceed 1.2 or 1.3, while the reduced pressure Pr (i.e., P/PC)
could be as high as those allowed by technological limits
(Mohamed and Mansoori 2002). For water and CO2, the
critical conditions of temperature (TC) and pressure (PC)
are 647K and 220 atm and 303.9K and 73.8 atm, respec-
tively (Evans 2002). Examples of the substances used as
supercritical solvents and their critical temperature and
pressure are shown in Table 1.
SFE was reported to be used for the extraction of
natural materials at a temperature close to ambient, there-
fore preventing the substance from thermal denaturation.
SFE is also a technique of solvent extraction; however, its
industrial application has been slow due to its sophisti-
cation (Tonthubthimthong et al. 2001). With the develop-
ment of the know-how and technology, SFE is nowadays a
well-established technique for extraction and separation
(Li et al. 2010).
612      J.M. Danlami et al.: A comparative study of extraction

Table 1 Supercritical solvents and their critical temperature and therefore precipitates into the trap. If a solid phase trap is
pressure (Ruhan et al. 2009). used, a supplementary rinsing pump is used to rinse the
analytes from the trap into the collection device (Nahar
Solvent   Molecular   Temperature   Pressure
and Sarkar 2005, Harlalka 2008). This extraction process
weight (g/mol) (K)
is preferred in situations dealing with low concentrations
      MPa   Bar of analytes strongly bound to the matrix (Chen and Ling
CO2   44.01   304.1   7.38   73.8 2000).
Water   18.02   647.3   22.12   221.2 Figure 5B shows the diagram of a dynamic extrac-
Methane   16.04   190.4   4.60   46.0 tion process. Dynamic extraction is usually conducted
Ethane   30.07   305.3   4.87   48.7
by bringing into contact a flow of extracting fluid at con-
Propane   44.09   369.8   4.25   42.5
Ethylene   28.05   282.4   5.04   50.4 stant supercritical pressure and temperature with a bed
Propylene   42.08   364.9   4.60   46.0 of particles that are ground to a suitable size to provide
Methanol   32.04   512.6   8.09   80.9 high surface area. If the extraction is diffusion controlled,
Ethanol   46.07   513.9   6.14   61.4 a dynamic phase beneficial as fresh extractant is con-
Acetone   58.08   508.1   4.70   47.0
stantly passed through the sample. An increase in the
flow rate also improves the efficiency of the extraction.
SFE involves five sequential steps: (1) penetration and A change in SC-CO2 flow rate has a significant impact on
diffusion of the solvent (e.g., CO2) within the solid matrix; the process, as observed in the extraction of artemisinin
(2) solubilization and breakdown of the components; (3) from Artemisia annua, whereby the artemisinin solubility
solute transport through the solid, with thin-film forma- was affected within the range 10–320 ml/min of CO2 (Xing
tion around the solid particles; (4) transportation of solute et al. 2003). Nevertheless, high solvent velocities are det-
from the external surface of the solid to the bulk of the rimental to extraction efficiency because of low loading of
fluid through a convective means; and (5) separation and the supercritical fluid and poor analyte trapping, whereas
discharge of the extract and solid. However, depending on very low velocities might cause plugging of the restrictors.
the mechanism of mass transfer, the extraction curve may A dynamic extraction could be a lot more exhaustive than
be associated with three extraction regimes: first stage of a a static extraction; therefore, impurities within the super-
constant extraction rate controlled by solubility, followed critical fluid become a major concern when using larger
by a decreasing extraction rate stage controlled mainly by amounts of fluid for extraction. The supercritical fluid
diffusion of solutes within the solid particle, and finally, contaminants can become concentrated at the collec-
the rate-limiting step, which involves internal diffusion tion device and could interfere with the extract analysis.
as a result of desorption of solutes. The constant rate will Another drawback associated with dynamic extraction
depend on the flow rate of the solvent (in the dynamic is the likelihood for coextraction of matrix components,
mode) and the characteristics of the adsorbed compound, as increased rates and amounts of supercritical fluid will
particularly its content within the solid matrix. In cases remove additional marginally extractable components.
of low concentration, the constant rate period might not There is also the risk of unwanted physical movement
exist at all (Bernardo-Gil 2013). of matrix components to the trapping device (collection
SFE can be accomplished using a static, dynamic, or vessel) at long dynamic extraction. Removal of analytes
coupled static/dynamic mode. A flow diagram of a static becomes a lot more probable from the trap as dynamic
SFE system is illustrated in Figure 5A. In static extrac- extraction time increases as a result of the blockage caused
tion, a fixed amount of supercritical fluid is pumped by the movement of the plant matrix (solid). In spite of
into the extraction vessel. After the desired pressure has these drawbacks, dynamic extraction is most favored by
been reached in the pump, valves V2 and V3 are closed. 90% of reported SFE applications (Nahar and Sarkar 2005,
The supercritical fluid circulates in a loop containing Harlalka 2008). Table 2 summarizes the advantages and
the extraction vessel by allowing the sample to soak at a disadvantages of the dynamic CO2 SFE extraction.
desired pressure and temperature for some period of time. A combination of static/dynamic SFE is gaining
After the extraction is completed, a valve (V5) at the outlet popularity, especially for situations where aggregate of
of the cell is opened to allow the analyte to be swept from solute and solvent must diffuse to the matrix surface to
the vessel through the restrictor and into the trap. Once the be extracted. The static mode extraction starts with no
supercritical fluid/analyte passes through the restrictor, flow through the system. As the extraction proceeds for a
the supercritical fluid decompresses to atmospheric pres- given period, the system is switched into a dynamic mode
sure and loses the bulk of its solvating power. The analyte by switching the valves. A fresh fluid enters the vessel,

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 J.M. Danlami et al.: A comparative study of extraction      613

A V1 V2
SCF 24 Pressure gauge
CO2 pump
Vent Oven
V4

CO2 Cylinder
V5 Back
Extraction pressure Trap
vessel regulator

V3
Modifier
pump
Heat exchanger

Solvent

SFX 200 Dynamic valve

B Chiller
Controller
CO2 Pump
CO2 Regulator

Heat
exchanger

Restrictor
fitting
Analyte valve Pressure
CO2 Tank
gauge
Extraction
chamber Needle
valve

Sample
collector Back pressure
regulator

Figure 5 A, Flow diagram of a static SFE system. B, Schematic diagram of dynamic SFE system.

Table 2 Advantages and disadvantages of dynamic CO2 SFE extraction (Gupta and Jae-Jin 2007).

  Advantages   Disadvantages

1.   The device can be assembled from   The method is affected by the mass transfer rate between the fluid and the solute. There is
easily available parts. always a possibility that the solute concentration has not reached its equilibrium value. In such
a case, the experiment should be extended by increasing the residence time of the fluid, to
ascertain that equilibrium has been reached.
2.   The sampling method is simple.   Heavy solutes can also clog the exit restrictor, which may cause the solute hold-up, resulting in
a lower solute collected in the trap than the equilibrium amount. In fact, most nonreproducible
solubility may be ascribed to erratic flow due to a plugged restrictor.
3.   Large amount of data can be   Entrainment of solute droplets can occur at high flow rates, resulting in more solute collection
obtained in a short time. in the trap than the equilibrium amount.
4.   Equilibrium and fractionation data   At higher pressures, if the density of SC-CO2 is higher than the solute, the solute floats and
can be obtained. is pushed out of the column, resulting in higher solute collection in trap compared to the
equilibrium amount.
5.   CO2 flow rate measurement can   When solute mixture is used, care should be taken not to deplete one of the components.
  be obtained with simple gas flow   If the solute phase undergoes phase transition, it can remain unnoticed unless a sapphire
meter at exit solute vessel is used.

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614      J.M. Danlami et al.: A comparative study of extraction
replacing the initial supercritical fluid that has been
exited through the restrictor to the trap. Combinations of
both static/dynamic cycles have been used for oil removal
from crushed peanut. The dynamic extraction yielded
approximately 25.4% recovery, while the static/dynamic
extraction gave 27.8% recovery (Megan et al. 2002, Nahar
and Sarkar 2005, Harlalka 2008).
The SFE extraction vessels are made from stainless
steel tube with automatic sealing thimbles or compression
end fittings. The vessel should be able to withstand the
generated pressure by the pump and should also be inert.
The function of each vessel must be carefully considered
in selecting the size, shape, and process holding vessels.
The vessel might require special designs, in some cases
to keep them clean and minimize plugging and contami-
nation. The size of a commercial analytical SFE extrac-
tion vessel might range from 0.1 to 2 dm3, as most sample
masses of SFE are  < 10 g. The amount of supercritical
fluid required to conduct a typical extraction depends on
several parameters; usually, three extraction-cell volumes
are required at least. The extraction cell is kept in an oven
to regulate the temperature. Since temperature affects
supercritical fluid density, any fluctuation in temperature
would lead to a change in density and, hence, the solvent
strength. In addition, higher temperatures can increase
the solubility of an added modifier and cause equilibria
complications (Nahar and Sarkar 2005).
As soon as the SFE plant is equipped with a number of
separators in series, fractionation of the extracts is feasi-
ble by operating the separators at dissimilar temperatures
and pressures. The possibility of this process is to induce
a selective precipitation of different compound families as
a function of their different saturation conditions in the
solvent. This process has been useful in the SFE of essen-
tial oils to separate them from coextracted cuticular waxes
(Reverchon and Marco 2006).
Most often, measurement devices are connected online
to the process using a continuous optical system through
which the analyte to be monitored is passed. Some systems
are connected to chromatographic [Gas chromatograph
(GC), High performance liquid chromatograph (HPLC), or
SFChromatograph] column and then analyzed. The devel-
opment of these analytical techniques has revolutionized
the analysis of fatty acids, and undoubtedly, the supercriti-
cal fluid chromatography technique is the most frequently
used. The packed column supercritical fluid chromatog-
raphy is a robust and easy phase chromatography ideally
suited for the analysis and purification of low to moderate
molecular weight, thermally labile molecules. Less polar
solvent or any molecule that is soluble in methanol is an
ideal candidate for supercritical fluid chromatography.
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Supercritical fluid chromatography is capable of
separating polar solutes readily. Several strong bases
that are difficult to separate by other techniques separate
rapidly with symmetrical peak shapes. Supercritical fluid
chromatography offers better speed and complimentary
selectivity to HPLC. The speed advantage of supercriti-
cal fluid chromatography, in comparison with HPLC, has
been illustrated in many case studies in food industries,
especially for speedy detection of food adulterants. Super-
critical fluid chromatography offers a wider range of
adjustments, enhanced sensitivity, and improved dynamic
range in comparison with HPLC. Supercritical fluid chro-
matography can also be used for preparative separations
at low cost per sample with low solvent consumption. The
gas-like properties of supercritical fluids allow for better
diffusivity, enhanced resolution, and the use of longer
columns. Supercritical fluid chromatography is also very
compatible with gas phase detectors often used in gas
chromatography (Jennife and Rui 2008).
The initial cost of SFE operations is high because
of the high fixed cost involved with the high-pressure
equipment commonly made up of expensive stainless
steel, which has been pointed out as a major drawback of
installing SFE industrial unit (Meireles 2008). Moreover,
appreciable mass transfer resistance encountered during
oil extraction and other natural compounds results in high
recompression cost of the recycled fluid (Rizvi 1998). On
the other hand, the operating costs are usually lower than
those of conventional extraction (Michel 2000, Sovová
and Stateva 2011). Thus, several large-scale units for the
SFE of solid natural materials, mainly for food ingredients
and phytopharmaceuticals, are operated worldwide and
are economically competitive.
Sample preparation methods based on the use of
compressed fluids, such as SFE and PLE, provide fast,
reliable, clean, and low-cost product/method that can be
used for routine analysis (Rosa and Meireles 2005, Pereira
and Meireles 2007a,b, Leal et al. 2009, 2010, Prado et al.
2009, Takeuchi et  al. 2009, Pereira and Meireles 2010,
Santos et al. 2010). However, SFE is useful for extraction
of both solid and liquid samples, whereas PLE is used for
solid samples. SFE is preferentially used to extract non­
polar compounds, whereas PLE can be used for both polar
and nonpolar compounds since all conventional solvents
can be used in this method.
Commercial SFE has been developed and marketed
throughout the world. Isco Inc., Applied Separations Inc.,
and Leco Corporation, USA, manufacture several types of
SFE units that offer considerable flexibility with respect
to sample size and experimental design (King 2002). The
commercial plants are located in the developed areas of

Europe, North America, and Asia. Green coffee beans
decaffeination was the first commercial SFE performed
in Germany by Hag AG. Subsequently, the hop extraction
process was developed in Australia. These commercially
successful applications led to improvements that enable
industrial scale-up.
2.5.2 Factors affecting SFE
The influence of pressure and temperature, modifiers, and
extraction time will be discussed. In addition to that, the
major aspect in SFE that needs attention is the extraction
optimization. Table 3 is a summary of important operat-
ing variables of SFE that should be optimized for a par-
ticular application to considerably improve the recovery
or extraction yield of fat and oils.
2.5.2.1 Effects of temperature and pressure
The solubility of oil in SC-CO2 is determined mainly by the
SC-CO2 density and the volatility of oil components (Kiri-
amiti et al. 2002). These two opposing effects of tempera-
ture on density and volatility lead to the well-established
crossover behavior of solubility isotherms. A temperature
increase may also result in breakdown of cell structure
and increases the diffusion rate of the oil in the particles,
therefore accelerating the extraction process. It is impor-
tant to consider that oil composition varies widely among
the different types of nut, and thus, differences in func-
tional groups and fatty acid compositions are responsible
for the differences in volatility, solubility in SC-CO2, and
crossover pressure. However, high pressure is generally
not recommended because increased repulsing solute-
solvent interactions ensuing from highly compressed
CO2 at high-pressure levels tend to induce complexity
in the extraction and difficulty in analysis. Second, the
saturation pressure of solute in supercritical fluid will
increase with the rise of temperature, which enhances
Table 3 Summary of operating variables affecting SFE (Cheah and Chin 2009).
  Sample preparation   Extraction parameters
1.   Sample mass   Supercritical fluid
2.   Comminution method   Pressure
3.   Homogeneity of sample   Temperature
4.   Water or moisture content   Flow rate
5.   Drying agent (type, ratio)   Modifier (type, amount)
6.   Vessel size   Static or dynamic extraction mode   Trap elution volume
7.   Packing density   Extraction time
8.     Restrictor temperature
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J.M. Danlami et al.: A comparative study of extraction      615
the solubility (Terada et  al. 2010). The extraction yield
improves significantly by increasing the pressure, as a
result of the increase in the solubility of the oil compo-
nents (Guan et al. 2007).
Grosso et  al. (2008) reported that the temperature
appears to increase the liberation of the monoterpene
hydrocarbons from the plant matrix after 10 min of extrac-
tion. Zhang et al. (2010) studied supercritical fluid of seed
oil from yellow horn. The extraction pressure was the
main parameter that influenced the extraction efficiency.
It was also observed that the oil yield increased signifi-
cantly with the increase in pressure at a given tempera-
ture, particularly at low pressure and temperature, and
that at a temperature of above 318K, the oil yield increases
at low pressure levels. As the pressure reaches a higher
level, there is a decrease in oil yield.
The influence of temperature on extraction is a lot
more difficult to predict than that of pressure due to its
two counter effects on the yield of oil. First, the increase
in temperature decreases the density of CO2, resulting in a
reduction in solvent power to dissolve the solute. Second,
the rise in temperature increases the vapor pressure of
the solutes, thereby bringing about the elevation of solu-
bility of oil in SC-CO2. Consequently, the solubility of the
solute may decrease, be kept constant, or increase with
rising temperature at constant pressure. This depends on
whether the solvent density or the solute vapor pressure is
the predominant factor.
2.5.2.2 Effect of modifiers
Modifiers, such as water, methanol, and ethanol, have
the advantage of inducing swelling of the matrix, there-
fore improving access to remoter matrix interior sites
(Kim et  al. 2008). It has been reported that the addition
of a modifier increases the yield of the analyte of inter-
est by up to threefold (Wang et al. 2001). The commonly
used modifier is methanol, which has excellent hydrogen
bond donating and accepting properties and is useful for
  Trapping
  Collection techniques
  Liquid trapping solvent/solid trapping agent used
  Trap size/solvent volume
  Collection temperature
  Trap elution solvent
  Temperature/flow rate
 
616      J.M. Danlami et al.: A comparative study of extraction
extracting polar analytes, although ethanol is generally
used (Kong et  al. 2009, Sánchez-Vicente et  al. 2009, Shi
et  al. 2009). Methanol-modified CO2 led to the recovery
of flavanone from osage orange tree root bark. This extra
flavanone was absent in the extracts obtained by the tra-
ditional solvent extraction techniques. Water (Kim et  al.
2008), as well as natural plant oils (Ciurlia et al. 2009, Shi
et al. 2009), has also been used as modifiers. The addition
of a modifier to a great extent can increase the complexity
of the SFE system. These include changes in the critical
conditions to ensure a homogeneous single phase of the
extracted fluid. Hence, a modifier is used only when an
increase in supercritical fluid density fails to extract the
natural materials of interest. However, poor yield might
still result despite the use of high extraction pressure and
modifiers. Yields of polyphenolic, glycosidic compounds
from hawthorne, marigold, and chamomile were shown
to remain low even at a high extraction pressure of 689
bar, with 20% ethanol in CO2 (Hamburger et al. 2004), and
hypericin yields also remained low despite the addition of
ethanol as a modifier (Catchpole et al. 2002).
The solubility of polar organic compounds in SC-CO2
is limited, and their extraction with SC-CO2 is not as
pure as possible. The addition of a nonpolar modifier to
SC-CO2 decreases the extraction efficiency. However, the
addition of a polar solvent (e.g., methanol) as modifier
compound enhances the extraction of components such
as FFAs, alcohols, and waxes by increasing the solubil-
ity of the analytes in CO2 (Ghasemi et al. 2007, Rial-Otero
et  al. 2007). Danh et  al. (2010) investigated the effect of
pressure, temperature, and amounts of added ethanol
on vetiver essential oil by using supercritical fluid. The
ethanol-modified supercritical fluid performed greatly
in producing high yields of vetiver oil with low pressure
extraction apparatus.
2.5.2.3 Effect of extraction time
The extraction is composed of three stages: rapid free
solute extraction, transitional phase of surface and inter-
nal diffusion, and slow extraction mainly based mostly on
the inner diffusion. The time consumed during the extrac-
tion stage depends on the solute solubility in SC-CO2 and
the particle size. Yin et al. (2005) reported that almost all
parts of seed oil were extracted in the first 90–100 min.
Safaralie et  al. (2010) also extracted essential oil from
valerian roots. The dynamic extraction was found to have
a dual effect (shortened the time and increased the yield)
on the extraction of valerenic acids compared with hydro-
distillation. Moreover, the dynamic CO2 extraction led to
an increase in the oil yield. That is possible due to the drag
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of a part of the extracted volatile compounds by CO2 from
the vessel collecting the desired constituents.
2.5.3 SFEs (CO2-SFE) of oil from numerous sources
CO2 is the most common supercritical fluid solvent used
and has been studied for its potential applications in
several fields, including the food processing industries
and lipid extraction (Zaidul et  al. 2007a,b), because of
its low critical temperature and pressure, low cost, wide
availability, and nonflammability (Berger et  al. 2000).
The CO2 used is essentially a by-product of industrial pro-
cesses, and its use as supercritical solvent is environmen-
tal friendly.
Supercritical fluid at its critical temperature and pres-
sure has shown unique properties entirely different from
those of either gasses or liquids under normal conditions.
CO2 has the ability to function as a chemical and also as
outstanding solvents for certain desired components
under an appropriate set of pressure and temperature
conditions. The final products obtained by SC-CO2 extrac-
tion (CO2-SFE) maintain their quality, and stability of ther-
mally labile natural components is guaranteed without
changing the bioactivity of natural molecules. CO2-SFE
has shown the possibility of being an alternative method
to both extraction and refining processes, particularly
for natural oils and bioactive compounds (Gracia et  al.
2009). The density and viscosity of supercritical fluids are
lower than those of liquids; however, diffusivity is about
two orders of magnitude higher than in typical liquids
(Brunner 2005, Selva et  al. 2008). Examples of physical
properties of the SC-CO2 and comparison made with other
liquid solvents are shown in Tables 4 and 5.
SC-CO2 conditions may be varied for selective extrac-
tion of antioxidant fraction with no residual aroma from
rosemary plants (Gupta et  al. 2012). It has been shown
that CO2 is used as a solvent for the selective extraction
of essential oils, fats, and oils and diterpene glycosides
from plants of medicinal interest under subcritical tem-
perature and pressure (Huie 2002). SC-CO2 behaves as
lipophilic solvent; however, it has an advantage over
liquid solvents. SFE produces products without artifacts
and a better retention of the original fragrance. Essential
oil extraction prefers low CO2 density of (0.25–0.50 g/cm3).
However, a higher CO2 density can be used for extraction
of non-oil compounds. The use of CO2 (and methanol as
cosolvent) to extract nimbin in an extractor built from a
piece of high-pressure HPLC tubing has been reported
(Tonthubthimthong et al. 2001). The effects of operating
conditions on extraction viz. CO2 flow rate, CO2 pressure,

Table 4 Comparison of properties of gas, liquid, and critical temperature and pressure of CO2 (Nurhan et al. 2003, Azizi 2007).
Region   Viscosity (g/cm s)
Gases (1 atm, 288–303 K)   (0.1–0.3) × 10-3
SC-CO2 Tc, Pc (304 K, 73.8 atm)   (0.1–0.3) × 10-3
Tc, 4 Pc (304 K, 73.8 atm)   (0.3–0.9) × 10-3
Liquids (288–303 K)   (0.02–0.3) × 10-1
Table 5 Comparison of physical properties of SC-CO2 with liquid solvents at 25°C (Ruhan et al. 2009).
  CO2 (200 atm, 328K)
Density (g/ml)   0.746
Kinematic viscosity (m2/s × 10-7)   1.00
Diffusivity of benzoic acid (m2 × 109)   6.0
extractor temperature, and weight of neem sample were
investigated. Nimbin extraction yields of approximately
0.35 kg nimbin/kg of nimbin seeds were obtained using
SC-CO2 extraction. The extraction yield was approximately
0.175 mg nimbin/g of neem seeds, where the neem seeds
were assumed to contain 0.5  mg of nimbin/g of neem
seeds. The best extraction conditions were found to be at
308 K, 23 MPa, and a flow rate of 1.24 ml/min. The sample
size was not found to affect the specific extraction rate
for a range of samples studied (Tonthubthimthong et al.
2001).
SFE conditions were optimized for extraction of active
ingredients from Curcuma zedoaria, and the density
of CO2 and the fluid volume passing through the plant
matrix were found to be factors increasing the extraction
efficiency, while increasing the temperature has little or
no effect on extraction efficiency (Huie 2002). The rate of
extraction of volatile active components like essential oils
from plant matrices by CO2-SFE appears to be governed
by analyte-matrix interaction instead of the bulk solubil-
ity of the analyte in the pure CO2 and the extraction rate
was found to increase greatly due to addition of an organic
modifier (Huie 2002).
The most extended use of SC-CO2 is in the decaffeina-
tion of tea, flavor extraction from herbs, aroma extraction
from juices, extraction of colorants, refinement of fats
and oils, extraction of antioxidants, deacidification of oil,
and inactivation of orange juice pectin esterase (Sahena
et al. 2009). A high variety of samples, types of materials,
target compounds, and procedures have been published
in the last years. A relatively new group of applications
that have been recently developed includes the extraction
and fractionation of carbohydrates by SC-CO2. This tech-
nique, which is massively employed, is not at first sight
the best option for this group of compounds, given the low
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J.M. Danlami et al.: A comparative study of extraction      617
  Diffusion (cm2/s)   Density (g/ml)
  1–4 × 10-1   (0.06–0.2) × 10-2
  0.007   (2–5) × 10-1
  0.002   (4–9)
  (0.02–0.2) × 10-4   0.6–1.6
  n-Hexane   Methylene chloride   Methanol
  0.660   1.326   0.791
  4.45   3.09   6.91
  4.0   2.9   1.8
polarity of CO2. However, with a relatively low amount of
polar entrainer, its usefulness has been demonstrated for
these applications (Herrero et al. 2010).
Extraction of grape seed oil by SFE with CO2 offers
great advantage regarding the efficiency of the method
(Gupta et  al. 2012). The oil obtained by extraction with
SC-CO2 is completely free of organic solvent, and the pro-
cessing time was lower than during conventional solvent
extraction. SC-CO2 extraction has also been applied for
extracting seed oils from fennel seeds (Reverchon and
Marco 2006). SFE has been demonstrated to be highly
effective than other techniques for the extraction of anti-
microbial compounds.
A clear trend in food and natural product analy-
sis, as well as in other fields of analytical science, is the
hyphenation of sample treatment procedures with ana-
lytical tools in order to produce effective online couplings.
Some of these couplings have involved the use of SFE. For
instance, SFE has been directly coupled to a CE (capillary
electrophoresis) instrument with fluorimetric detection
to effectively carry out the cleanup of the sample and the
direct CE analysis of riboflavin from chicken liver (Herrero
et al. 2010).
Temelli (2009) reported and classified specialty
oils that have been extracted from various seeds and
nuts using SC-CO2. The major advantage of the SC-CO2
extraction technique for specialty oils is preserving the
distinctive flavor and aroma, whereas volatile aroma
compounds are usually lost in traditional and ancient
solvent extraction processing. Specialty oils contain high
levels of bioactive materials, like polyunsaturated fatty
acids, tocopherols, tocotrienols, carotenoids, phytoster-
ols, and squalene. These components above play posi-
tive roles in human health as precursors to vitamins A,
E, and K. Due to the general public awareness along with
618      J.M. Danlami et al.: A comparative study of extraction

Table 6 Summary of oil extracted using SC- CO2 and other methods of extraction for selected oil.

S.   Examples   Extract   Solvent   Extraction methods   Time, yield   Reference

No. (temperature, °C;
pressure, MPa)

1.   Hippophae rhamnoides L.   Seed oil   CO2   SFE (40, 25)   –   Yin et al. 2005
2.   Valeriana officinalis L. roots  Essential oil   CO2   SFE (37, 24.3–25)   –   Safaralie et al. 2010
3.   Plant material   Essential oil   CO2   SFE (ND, ND)   –   Araus et al. 2009
4.   Yarrow flowers   Essential oil   CO2   SFE (40–60, 10)   –   Bocevska and Sovová
2007
5. Vetiveria zizanioides root
    Essential oil   CO2   SFE (50, 190 bar)   –   Danh et al. 2009
6. Citrus reticulate peel
    Oils   CO2   SFE (60, 10)   –   Danielski et al. 2008
7. Coffea arabica beans
    Green coffee oil   CO2   SFE (70, 15.2)   –   de Azevedo et al. 2008
8. Valeriana officinalis L.
    Essential oil   CO2   SFE (37–61, 15–30.4)   –   Safaralie et al. 2008
rhizomes
9.   Carqueja   Carqueja oil   CO2   SFE (30–40, 100–300   –   Silva et al. 2009
bar)
10.   Chrysobalanus icaco   Essential oil   CO2   SFE (85.15,20)   –   Vargas et al. 2010
11.   Salvia mirzayanii   Essential oil   CO2   SFE (35, 35.5)   –   Yamini et al. 2008
12.   Patchouli   Essential oil   CO2   SFE (40,14)   –   Donelian et al. 2009
13.   Palm kernel   Palm kernel oil   CO2   SFE (45.2–85.2, 20.7)   –   Zaidul et al. 2007a,b
14.   Juniperus communis L.   Essential oil   CO2   SFE (45,11.8)   –   Orav et al. 2010
15.   Salvia lavandulifolia L.   Essential oil   CO2   SFE (40, 90 bar)   –   Langa et al. 2009
16.   Nepeta persica   Essential oil   CO2   SFE (45, 20.3)   –   Khajeh et al. 2010
17.   Satureja hortensis   Essential oil   CO2   SFE (72.6, 35)   –   Khajeh 2010
18.   Artemisia sieberi   Essential oil   CO2   SFE (50, 30.4)   –-   Ghasemi et al. 2007
19.   Rose hip seed   Oil   n-hexane   Sox (Rfx: 1–25)   3 h, 48.5 g/kg   Szentimihulyi et al.
2002
      n-hexane   UAE (Rfx: 1–25, 69°C)   1 h, 32.5 g/kg  
      n-hexane   MAE (Rfx: 1–35, 40°C)   30 min, 52.6 g/kg  
      CO2   SFE (35°C, 250 bar)   1 h 20 min,  
57.5 g/kg
      CO2: propane   SFE (28°C, 100 bar)   35 min  
20.   Cuminum   Essential oil   Solvent-free   MAE   30 min   Wang et al. 2006
  Cyminum     extraction      
21.   Olive seeds   Edible oil   Hexane   MAE   20–25 min   Stashenko et al. 2004
22.   Cyperus rotundus rhizomes   Essential oil   Methanol   PLE (140°C, 1000 Psi)   10 min   Tam et al. 2007
          Fv: 60%  
23.   Momordica charactia   Charantin   Ethanol or   PLE (100°C, 10 MPa)   60 min   Pitipanapong et al.
acetone 2007
24.   Lysimachia clethroide   Flavonoids   50% acetonitrile   PLE (100°C, 1500 psi)   25 min   Jiang et al. 2007
          Fv: 70%  
25.   Derris elliptica, Derris   Rotenone   Chloroform   PLE (50°C, 2000 psi)   3 days   Sae-Yun et al. 2006
malaccensis root, stem
26.   Capsium peppers   Capsaicinoids   Methanol   PLE (200°C, 100 atm)   5 min   Barbero et al. 2006
27.   Panax notoginseng   Ginsenosides   Methanol   PLE(150°C)   –   Wan et al. 2006
28.   Piper gaudichaudianum   Terpenes, fatty   Petroleum ether   PLE (85°C, 1500 psi)   10 min   Péres et al. 2006a,b
leaves acids, vitamin E or ethanol

food demand, industries are continuously searching for
such oils that are naturally extracted. Meanwhile, SC-CO2
extraction has been demonstrated in the literature as the
best method for bioactive and lipid components (Bravi
et al. 2007, Glišić et al. 2007, Martínez et al. 2008, Shi et al.
2010).
SC-CO2 has been used extensively to extract oil as
well as fatty acid from numerous seeds. Essential fatty
acids like linoleic acid are also necessary for human
metabolism and cannot be synthesized in the human
body. Essential fatty acids should be provided externally
from the diet. These fatty acids play a vital role in cell

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 J.M. Danlami et al.: A comparative study of extraction      619

Table 7 Summary of advantages, disadvantages, and applications of extraction methods.

Methods   Advantages   Disadvantages   Applications   References

Solvent   Several extractions can be   Large amount of extractant   Analysis   Eskilsson and Björklund 2000, Chemat et al.
extraction performed in parallel. waste. 2008, Sehana et al. 2009, Kothari et al.
2012, Al-Zahrani and Putra 2013, Han et al.
2013, Perez et al. 2013, Yan 2013
  Required little training   Extraction is limited extractant   Environmental  
and difficult to automate. remedy,
antioxidant
  Can extract more sample   Temperature gradient heating.   Phynolic  
mass than other methods compounds
can
    Hazardous and flammable   Antioxidant  
liquid organic solvent.
    Potential toxic emissions    
during extraction.
    Costly and high purity solvents    
are required.
    Cleanup step is needed.    
Microwave   Moderate investment   Energy can result in lipid   Carotenoids   Eskilsson and Björklund 2000, Chemat et al.
assisted oxidation. 2008, Li et al. 2012, Upadhyay et al. 2012,
extraction Bajpai et al. 2013, Cardoso-Ugarte et al.
2013, Lei et al. 2013, Mohamadi et al. 2013,
Périno-Issartier et al. 2013, Shah and Rohit
2013, Shao 2013
  Loss of volatile compound   No high solution temperature   Gossypol  
is avoidable.
  Air-borne contamination   Single step excludes solvent   Biological active  
is avoided. addition. compounds
  No provision of hazardous   Vessel should be cooled to void   Antioxidative  
fumes loss of volatile component. compounds
      Phenol extraction  
Ultrasound   Consumes small amount   Deleterious effect of ultrasound   Defoaming   Wang et al. 2012, Ahmad-Qasem et al.
Assisted of fossil energy energy on active constituents 2013, Chavan and Singhal 2013, Gil-Chávez
extraction et al. 2013, Golmohamadi et al. 2013, Shah
and Rohit 2013
  Low investment cost   Large solvent volume   Extrusion  
    Filtration step required   Fermentation  
    Repeated extractions may be   Heat transfer  
required.
      Microbial  
inactivation
Pressurized   User friendly   High cost of investment   Extraction of   Eskilsson and Björklund 2000, Chemat et al.
liquid organic pollutants 2008, Plaza et al. 2012, Oliveira et al. 2013,
extraction Shah and Rohit 2013, Tierney et al. 2013
  Safe and rapid extraction   For analytical use only   Cocaine extraction  
  Works under high     Natural products  
temperature and pressure steroids
to increase efficiency
Supercritical  Fast extraction   Many parameters to optimize   Analytical   Eskilsson and Björklund 2000, Chemat et al.
fluid approach 2008, Sunarso and Ismadji 2009, Lozowski
extraction 2010, Occhipinti et al. 2013, Wejnerowska
et al. 2013, Zhou et al. 2013, Zhu et al. 2013
  No filtration is required.   Higher technical complexity   Waste  
detoxification
  Automated system   Inadequate theoretical/   Aromas  
practical interest
  No hazardous waste   Risk of volatile analyte loses   Colorants  
  Fractionation capabilities   Risk of system clogging    

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620      J.M. Danlami et al.: A comparative study of extraction
membrane formation and also proper development and
functioning of the brain and nervous system. Hormone-
like substances like eicosanoids produced by essential
fatty acid are accountable for regulating blood pressure
and also viscosity, vasoconstriction, immune, and inflam-
matory responses (Sánchez-Vicente et al. 2009). It has also
been demonstrated that fatty acid deficiency is related to
many human diseases. Fatty acid consumption has health
advantages like reduced inflammatory diseases. SFEs of
oils from numerous sources are shown in Table 6.
3 Conclusions
The significance of extraction of plant materials such as
foods, fragrances, flavors, nutraceuticals, fat, oils, etc.,
prompts continued research for economically and ecologi-
cally extraction techniques, such as MAE, UAE, PLE, and
SFE. Traditional solid-liquid extraction requires a large
amount of solvent and is also time consuming. The quan-
tity of solvent used increases operating costs and also
causes environmental degradation. For these reasons,
other techniques were developed as an alternative
extraction method to overcome the shortcomings of the
conventional methods, providing advantages to extrac-
tion time, solvent consumption, and reproducibility and
extraction yields. This review presents the principles and
mechanisms of various extraction techniques for better
understanding of the processes involved and summarizes
the potential of these techniques in the extraction of oil
from plants and seed materials. Emphasis was placed on
extraction parameters, such as temperature and pressure,
modifiers, and extraction time for complete recovery of
analytes from plant matrices using SFE. A comparative
analysis of the traditional Soxhlet extraction with other
extraction techniques was also presented.
The prospect of MAE, UAE, PLE, and SFE for the
extraction of volatile components, fats, and oils from
plants appears bright in light of the wide area of appli-
cations. Methods such as SFE, MAE, and UAE are better
suited for the extraction of heat-labile compounds, which
is not the case with the conventional methods. The
former are more promising for industrial applications
due to the enhanced efficiency, specificity, and selec-
tivity. At present, both analytical and industrial-scale
commercial productions of MAE, UAE, and SFE are avail-
able for industrial used throughout the globe, whereas
PLE is used only for analytical purposes. And lastly, the
eco-friendly nature of only the CO2-SFE technique is of
great importance. Table 7 summarizes the advantages
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and disadvantages of the different extraction methods
reviewed in this paper.
Further research is needed to overcome the disadvan-
tages and improve the design and scale-up of these new
extraction methods to enhance their lab scale and indus-
trial applications.
Acknowledgments: The authors acknowledge the
Research University Grant (GUP) of Universiti Teknologi
Malaysia (Grant no. 03H08) for financial support.
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Jibrin Mohammed Danlami received his bachelor’s and master’s
degrees in chemical engineering from the Federal University of
Technology, Minna, Nigeria. He is a PhD student at the Centre of
Lipid Engineering and Applied Research (Clear), Faculty of Chemical
Engineering, at UTM. His research is in the field of supercritical fluid
extraction.
Agus Arsad is a senior lecturer in the Department of Polymer
Engineering, UTM. He was awarded a PhD in polymer engineer-
ing from UTM in 2010. He has published several research papers
and conference proceedings on polymer green composites and
nanocomposites, polymer rheology, and chemical process separa-
tion. His research interests include chemical separation, polymer
nanocomposites, and polymer rheology.
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Muhammad Abbas Ahmad Zaini received his PhD from Chiba
University, Japan, in 2010. He currently serves as a senior lecturer
at the Department of Chemical Engineering, UTM Johor Bahru. He
is actively involved in research on the conversion of agricultural
wastes into activated carbons/low-cost adsorbents and their
applications in oil, heavy metal, and dye removal from water. His
research interests also include liquid-phase adsorption, gas-phase
absorption, and supercritical fluid extraction.
Hanizam Sulaiman is an associate professor of Polymer Engineering
at the Department of Polymer Engineering, UTM. He received his
master’s of science degree in polymer technology at Loughborough
University of Technology, UK, in 1990. Green solid fuel development
from plastic wastes is his main research interest. He has developed
a quick and simple way to predict the heating value of Malaysia’s
municipal solid waste. His research interests also include industrial
and solid waste management and laboratory system design.