Review

Optimization Methods for the Extraction of Vegetable

Oils: A Review
Divine Bup Nde * and Anuanwen Claris Foncha
Department of Nutrition, Food and Bio-resource Technology, College of Technology, University of Bamenda,
P.O. Box 39, Bamenda, Cameroon; [email protected]
* Correspondence: [email protected]; Tel.: +237-675417724

Received: 25 December 2019; Accepted: 30 January 2020; Published: 8 February 2020

Abstract: Most seed oils are edible while some are used generally as raw material for soap
production, chocolate, margarine, and recently in biodiesel formulations as potential candidates
capable of replacing fossil fuels which are costly and destructive to the environment. Oilseeds are a
green and major reservoir which when properly exploited can be used sustainably for the
production of chemicals at both the laboratory and industrial scales. Oil extraction is one of the
most critical steps in seed oil processing because it determines the quality and quantity of oil
extracted. Optimization of the extraction conditions for each extraction method enhances yield and
quality meanwhile a carefully chosen optimization process equally has the potential of saving time
and heat requirements with an associated consequence on cost reduction of the entire process. In
this review, the techniques used to optimize oil extraction from plant materials which can be
consulted by stakeholders in the field are brought to focus and the merits and demerits of these
methods highlighted. Additionally, different types of optimization techniques used for various
processes including modeling and the software employed in the optimization processes are
discussed. Finally, the quality of the oil as affected by the methods of extraction and the
optimization process used are also presented.

Keywords: oilseeds; oil extraction; experimental designs and optimization; polynomial modelling;
optimization software

1. Introduction
Many plants contain extractible oils that have for centuries been used either as food or in
cosmetic formulations [1]. Recently some of these plant bearing oils have caught the attention of
researchers as a source of renewable energy especially in bio-diesel fuel production [2,3]. Oil content
of oleaginous seeds, nut, kernel, or fruit pulps varies between 3% and 70% of the total weight and
has similar chemical structures to animal fats [4]. The benefits that accrue from oilseed processing
and sales to individual or grouped farmers, companies, and even to national economies cannot be
overemphasized because two of its major products oils and meal or cake are both of great
commercial value. For example, in developing countries such as Malaysia, Cameroon, and Ivory
Coast there are considerable sections of the population that source their livelihoods principally from
palm oil processing and sale. Statistics show that global production of vegetable oil has steadily
increased from about 90.5 million metric tons in 2000/2001 to 207.5 million metric tons in 2019/2020
and these trends are expected to continue in the future [5]. Major plant oil sources of commercial
importance out of the 40 documented ones that contain edible oils include soybean, sunflower,
groundnuts, rapeseed, coconut, and oil palm [6]. Other oilseeds of less commercial importance
which are however highly cherished because of the important roles they play in one or more of the
following processes; soap production, chocolate, margarine, and biodiesel production etc. include
castor, safflower, shea, neem, and tung oils etc. Amongst the many unit operations involved in the

Processes 2020, 8, 209; doi:10.3390/pr8020209 www.mdpi.com/journal/processes

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processing of oils from oilseeds, extraction remains one of the most critical steps because it
determines the quality and quantity of the oil extracted. Initial oil content is a major factor that
determines the choice of grain processing and extraction methods for the various oil seeds [7].
Although extraction methods especially for the more conventional oilseeds are known, there
has been a continuous quest by researchers to improve extraction yields. One proper way of
improving extraction yields is to optimize the extraction conditions for each type of extraction
method and oilseed because optimum yield will vary with these factors. Apart from enhancing
yields and quality, a carefully chosen optimization process equally has the potential of saving time
and heat requirements with an associated consequence on reducing the cost of the entire oil
extraction process. A number of optimization methods for the extraction of useful components from
plant material have been documented in the literature [1,3,6]. While many researchers have
embraced the investigation of nonconventional oils obviously for the multipurpose uses of the oil,
there has not been a corresponding effort in documenting published results on oilseeds in the form
of reviews that could be available to stake holders for consultation at all times. The few reviews on
this subject have lightly discussed the methods of extraction without laying emphasis on types of
oilseeds, optimization methods of the extraction processes, modelling, as well as the influence of
the extraction and optimization methods on the quality of the extracted oil [8–10]. Consequently, to
the best of our knowledge, there is no comprehensive review on the various techniques used for
optimizing oil extraction from plant material. This work therefore presents a review on techniques
used to optimize oil extraction from plant material which can be consulted by stakeholders in the
field. The work summarizes the general methods of oil extraction from oilseeds, followed by the
different types of optimizations techniques used for the various extraction processes including
modelling and the software used in the optimization process. The last section of the work is centered
on the oil quality as affected by the extraction methods and the optimization process used.

2. Oil Extraction Methods

The process of separating triglycedrides from oilseeds is referred to as extraction. This is
possible through a variety of chemical, biochemical, and mechanical techniques in order to
maximize yields while minimizing alterations on the quality of the product [11]. It is the most
important part of oil processing and depends on the part that contains the oil, which is the kernel,
the seed, or the pulp [12]. The separation of bio-active compounds of interest in different industries
such as food and pharmaceutical usually employs the use of large amounts of solvents (water,
n-hexane, ethanol, chloroform, methanol, petroleum ether, etc.). Over the last decades researchers
have concentrated lots of efforts on the design of efficient and more sustainable methods of
extraction which are less detrimental to the environment [1–15]. Extractions have moved from the
conventional solvent and mechanical extractions to improved nonconventional techniques such as
Supercritical Fluid Extraction (SFE) and extraction assisted by ultrasound (UAE) and
microwaves(MAE) [16–18].Grinding is a very essential operation in the preparation of materials for
oil extraction irrespective of the method that follows because when carefully controlled it can lead to
the achievement of high oil yields and positively influences downstream operations [19].

2.1. Mechanical Extraction (ME)

Mechanical extraction is one of the oldest methods used for oil extraction. In principle, the seeds
are placed between barriers where the volume available to the seed is reduced by pressing thereby
forcing oil out of the seeds [20].For application in rural areas, mechanical extraction is habitually
used because it has a lower initial investment cost and does require highly trained personnel to
operate the machines. The quality of oil obtained by this method is most often measured as a factor
of its acid value, phosphorus content, water content, and iodine value [3]. Advantages of mechanical
extraction include the production of good quality oil and the possibility of the use of its cake
compared to when extraction is done in solvents. Oil extraction by mechanical presses is the most
common and entails the use of either hydraulic presses or screw presses driven by a motor [2,21].
Even though mechanical pressing is efficient, it usually results in very low oil yield [3].The
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advantages of the screw press over the hydraulic press are its slightly improved yields and its ability
to be adapted for continuous processing. Heriawan et al. [22] studied a screw configuration of four
types of screws; transport, forward, reserve, and idle screws and two types of barrel filters for the
extraction of oil from Nyamplung Seeds (Calophyllum inophyllum L.) and concluded that it is necessary
to configure mechanical extractors per the seed material used because it can greatly impact the yield.
Mariano et al. [23] (2017), studied a mechanical screw press powered by a 2.2 kW electric motor to
study the influence of temperature (50 and 70 °C), rotational screw speed (22 and 32 rpm), and seed
pretreatment (seeds heated at 50 °C in an oven compared to unheated ones) on tobacco oil yield. An
optimum oil yield of 73.38% ± 0.307% (w/w) was obtained with heat treated samples at 70 °C and 32
rpm. In addition to temperature, Gikuru and Lamech [24], also studied the effect of compression
pressure and duration of applied force on the extraction yield of soybean oil using the traditional
optimization method of keeping some factors constant while varying one at a time. The results
showed an increase in the process parameters leads to an increased yield but there exist an optimum
bulk temperature which should not be exceeded in order to maximize oil yield. The study also
showed that there is a linear relationship between oil yield and both the magnitude of expressing
force and the duration of its application.

2.2. Conventional Solvent Extraction (CSE)

The conventional solvent extraction (CSE) process is amongst other factors based on the ability
of the solvent to dissolve oils and to extract them from the seeds. Therefore, the solvent must be able
to solubilize the oil for an efficient extraction. It is the most commonly used method usually carried
out either as a batch or continuous process. The three major steps involved in solvent extraction are
oilseed cleaning and conditioning, oil extraction, and separation of the miscella. Crude oil and meal
quality depend mostly on type of solvent used, reaction temperature, and type of pretreatment
given to the oilseed [25,26].The solvent-extraction method is preferable because it is cost efficient and
easy to use [18]. Bhuiya et al. [2] studied the oil extraction process from beauty leaf seed of
Australian origin and observed that the solvent extraction process was more reproducible, with
relative ease of seed preparation and did not require extensive training compared to the mechanical
extraction method. Jahiru et al. [27] compared the use of screw press mechanical and solvent
extraction methods of oil from beauty leaf and also concluded that the solvent method was superior
to the mechanical. The method however requires an extra refining step or process to obtain oil of
required quality [28]. CSE has a 90%–98% oil recovery rate but requires high energy, high
investments, and the solvent most often used (hexane) is hazardous and can cause health problems
with prolonged exposure [29–31]. Balaji et al. [26] reported that ethanol is more effective in the
extraction of oil from Tamarindus indica compared to n-hexane, petroleum ether, chloroform,
methanol, chloroform, methanol (2:1v/v), and iso-propanol and recommended the use of ethanol; a
safe and green solvent, in place of other solvents. Guilherme et al. [32] using subcritical propane
obtained more yield as opposed to pressurized ethanol under similar conditions. Despite the
shortcomings of hexane as an oil extraction solvent it is still being used in research and in some oil
process plants. For example, Haitham et al. [33] reported higher oil extracting yields from sesame
seeds with n-hexane (37.03%) compared to chloroform (6.73%) and acetone (4.37%).Temperature
increases diffusivity and solubility of oil which consequently improves the extraction rate [34].

2.2.1. Enzyme Assisted Extraction (EAE)

Plant cell walls are made up of lignocellulosic, and other polymers intertwined with each other,
which provide a barrier to extraction of its components [35]. Enzymes are used for the digestion of
these cellular materials and disruption of pores as a pre-extraction step which eases the diffusion of
the oil into the extraction medium [36,37]. Some of the most effective enzymes used are from the
fungus Trichoderma [38]. The choice of enzyme used depends on the structure of oilseed, enzyme
composition, type of enzyme, experimental conditions, etc. Cellulases, hemicellulases, and
pectinases, are commonly used during EAE to hydrolyze and degrade the cell wall thus improving
the release of intracellular content [39,40]. EAE are used by oil industries because they are site
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specific and operate at low temperatures [30]. Farah et al. [41] studied the effect of different enzymes
(cellulose, amylase, and cellulose+amylase) at different temperatures (35, 50, and 65 °C) and
extraction times (8, 16, and 24 h) on the yield of onion oil. The best yield of 18.38% was obtained from
samples extracted using a combination of amylase and cellulose at 65 °C for 16 h. Mai et al. [42] also
support the idea that a combination of enzymes leads to a better extraction. Even though the use of
single enzymes (protease, cellulose, pectinase, and α-amylase) led to a significant increase in the
quantity of oil extracted from gac (Momordica cochinchinensis Spreng.) fruits compared to the control;
a combination of all four enzymes in equal proportions gave a higher yield compared to when the
enzymes were used singly. Ferreira et al. [43] reported similar trends when they used four different
commercial enzymes separately and in combination, in the extraction of oils from the pulp of
Euterpeoleracea fruit. Despite some of these recorded successes with enzyme extractions, it is worth
noting that Anwar et al. [44] reported a lower yield for enzyme extraction (35.2%–38.0%) compared
to the conventional soxhlet extraction (42.6%) in a study with viscozyme, feedzyme, and kemzyme
assisted cold press extraction of oil from flaxseeds. This lower yield was attributed to the low
extraction temperatures probably because the most suitable temperature range for most enzymes
used for oil extraction is 40–55 °C [45]. Sharma et al. [46] reported a significant effect of temperature
on extraction yields of peanut oils at 40 °C which however dropped significantly when temperatures
were reduced to 37 °C. The drop was associated with a possibility of enzyme thermo-inactivation.
Danso-Boateng [47] also reported maximum oil extraction yields from sunflower kernel when
treated with a combination of steam explosion and viscozyme compared to CSE. Lower seed
material to water ratios can lead to reduced oil yields because the mixture will be too viscous and
difficult to homogenize and an excessive amount of water in the mixture would inevitably lower the
concentration and the hydrolysis efficacy of the enzyme [48]. Shah et al. [49] reported a suitable 1:1
solid to liquid ratio during the extraction of oils from Jatropha curcas L. seed kernels; reducing the
volume of t-butanol by half reduces the oil yield whereas doubling the volume did not have any
significant effect on the quantity of oil extracted. In order to assess the effect of pH on EAE of oil
from Pistacia khinjuk using protease and α-amylase, Ahmadi and Karimi [30] performed extractions
in the pH range 4–9 by adding desired amounts of HCl 0.1 N or NaOH 0.1 N into the slurry. The
results indicated that the oil recovery from the seeds using α-amylase in an aqueous medium
increased with an increase in pH while using protease enzyme, there was an initial increase in oil
recovery with an increase in pH which decreased slightly afterwards. In the production of shea
butter from shea nuts the pH range of 4–6 was found suitable in the presence of crude Pectinase and
commercial Pectinex but at very low or higher pH values, the produced oil had high viscosity
making separation by centrifugation very difficult, which was reflected in the low quantity of oil
recovered [50].

2.2.2. Ultrasound Assisted Extraction (UAE)

Ultrasound is a special type of sound wave beyond human hearing, with frequencies ranging
from 20 to 100 MHz [51]. Advantages of UAE include shorter extraction times, low energy
demands, and high extraction efficiency [16,52]. UAE is mainly attributed to the behavior of
cavitation which brings about the formation and growth of bubbles and its subsequent collapse.
The result of this collapse are physico-chemical and mechanical effects which provoke disruption of
material matrix, facilitating release of extractable compounds and aiding the movement of the
solvent into the sample thus increasing the release of target compounds from matrix into the
solvent [53]. Even with the advent of some other novel techniques of extraction such as
microwaves, UAE is preferred by some researchers because among other factors it is highly efficient
and saves time [54]. Wang and Wei [55] demonstrated that an increase in ultrasonic power led to an
increase in oil yield that, however, dropped significantly when ultrasonic power exceeded 90 W
(optimal ultrasonic power). It was explained that the oscillation rate of the solvent and oil increased
at higher ultrasonic power thereby facilitating the dissolution of seed oil. At ultrasonic powers
greater than 90 W, the cavitation produced by the ultrasonic waves does not only disrupt the cell
wall, but also damages the molecular structure of the seed oil, leading to a decrease in extraction
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rate. In an ultrasonic comparative assessment of biodiesel production from rapeseed, Ibiari et al. [56]
showed that using ultrasound assisted soxhlet extraction reduces extraction time by about 62%, but
the percent recovery was slightly lower than that of the conventional soxhlet extraction. This low
recovery rate was attributed to the high frequency (800 KHz) ultrasound employed. Extraction time
also affects yield as demonstrated by Lin et al. [57] who obtained an optimum yield of 86.5% for
hempseed oil extraction after 30 min. There was a significant increase in oil extraction yield as
extraction time increased from 15 to 30 min but after 30 min there was a significant drop in the oil
due probably to destruction of the cell material as earlier explained. Rosas-Mendoza et al. [58]
reported a 10% increase in yield for UAE during extraction of chia seed oil compared to 69.2% for
soxhlet extraction. Moreover, the researchers reported gains in extraction time because optimum
yield was achieved at 60 min for UAE while the same yield was obtained at 90 min for solvent
extraction. Isopencu et al. [59] optimized ultrasonic intensity (UI), temperature, and time in the
extraction of sea buckthorn oil. For optimized extraction, operation conditions were 13.77 W/cm2 UI,
40 °C, and 10 min extraction time for UAE. These results were compared to MAE parameters of
microwave power, time, and solid/liquid-ratio variables. The 225 W microwave power, 15 mL/g
solid/liquid ratio, and 20 min extraction time were the optimum conditions necessary to obtain a
yield of 87.4% ± 0.44%. The results showed that maximum yields for UAE were obtained in half the
time required for microwave assisted extraction (MAE). Yousuf et al. [60] demonstrated that in the
UAE of soybean oil, increase in power, sonication time, and solvent volume all had an increasing
significant effect on oil yield. These studies corroborate that of Wang and Wei [55],that assert that
increasing sonication time disrupts the cell wall and increases the interaction region between the
solvent and the material thereby increasing the amount of oil extracted. As the ultrasonic power
increases, the temperature and pressure within the bubbles of the solvent cause the breakdown of
these bubbles; this violent shock boosts the permeation of the solvent into the cell tissues and speeds
up the intracellular product discharge into the solvent. Additionally, with increasing solvent volume
there is an increase in the concentration difference of the oil in the seed material and the solvent
which aids mass transfer.

2.2.3. Microwave Assisted Extraction

Microwave assisted extraction (MAE) is one of the most recent and attractive alternative oil
extraction methods [61]. The protein material is denatured during microwave treatment leading to
an improved extraction [62].The rapid heating and destruction of biological cell structure by the
microwave ensures effective extraction within a short time requiring small amounts of solvent and
produces high quality oil [63–65]. Another important advantage of this process is the lower energy
requirement which decreases environmental impact and financial costs [58]. The mechanism of MAE
is attributed to ionic conduction and dipole rotation resulting from the effect of the microwaves on
the molecules of the material undergoing processing. Ionic conduction caused by the electrophoretic
migration and the dipole rotation of realignment of ions under an applied electromagnetic field
results in an increase in temperature of the extraction medium [28,66]. MAE is greatly influenced by
the solubility of the compounds of interest in the solvent, partition coefficient, mass diffusivity, and
the dielectric properties of the feedstock and the solvent [59]. Mgudu et al. [66] investigated the
effect of the microwave treatment on the yield and quality of the oil obtained from castor beans and
showed that the microwave treatment gave optimum yields of44.34% at a power of 280 W after 120
s. Mosquera et al. [67] also reported that a better quality palm oil with a lower unsaturated fatty acid
content even though a lower yield was obtained from the MAE process compared to expeller press
and solid-liquid extraction. Taghvaei et al. [68] reported a MAE yield of 32.6% compared to 34.7%
obtained from the soxhlet extraction after3.5 min and 16 h extraction time, respectively. Even though
MAE has been proven to extract several valuable phytochemicals, the thermal character of the
method makes it unsuitable for the extraction of polyunsaturated fatty acids (PUFAs) due to their
high vulnerability to oxidation and degradation [60]. Nde Bup et al. [69] also used MAE for the
extraction of sheanut butter, where they reported substantial gains in extraction time and reduction
in the quantity of solvent used compared to CSE. They reported an optimum yield of 31.6% after
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heating for 23 min at 75 °C and with a solvent/solute ratio 4:1 as opposed to 10 h, 65 °C, and a
solvent/solute ratio of 10:1 for solvent extraction

2.3. Supercritical Fluid Extraction (SFE)

SFE separates components from the matrix with the use of supercritical fluids. This method is
sometimes referred to as the supercritical carbon extraction method [70]. Solvents used in this
method include compressed gases such as ethane, propane, ethylene, dinitrogenoxide, and carbon
dioxide [71]. Carbon dioxide with properties of 10–50 MPa pressures and 35–80 °C temperatures
[72] is the most frequent solvent used because it has a relatively low critical temperature (31.1 °C), is
nontoxic, nonflammable, with good solvent power, low viscosity, high diffusivity, can be easily
removed from the product (does not leave organic solvent residues), and is readily available at low
cost [73–75]. SFE involves heating the solvent to above its critical point and at a pressure above 1100
psi. The rate at which this it is pumped through the sample is between 10 and 40 volumes [76]. SSFE
is sometimes preferred because it avoids the coextraction of impurities (heavy metals and organic
derivatives) in preference to the extraction of low polar lipid compounds [77]. Together with the
supercritical carbon dioxide (SC-CO2) other solvents usually referred to as cosolvents (e.g.,
methanol, ethanol, isopropanol, and acetone) can also be used in SFE. These cosolvents come most
often to boost the poor polarity of SC-CO2 and to increase its ability to solvate the analyte of interest
[78]. The carbon dioxide used can be recycled, thereby reducing energy consumption and increasing
the overall sustainability [79]. Unlike other methods such as CSE, UAE, and MAE that require
thermal treatment after extraction, the separation of supercritical carbon dioxide from the extracted
oil occurs by simple depressurization [80]. Bhupesh et al. [81] showed that in the extraction oil from
sunflower seeds, yield increased with the increasing temperatures at 40 MPa and decreased with
increasing of temperatures at 20 MPa. They also noted that the effect of pressure was highest at
temperatures of 70 °C and lowest at 40 °C and suggested the use of higher temperatures and lower
pressures. At higher temperatures and their corresponding pressures, the plant tissues are softened
thereby increasing the solubility of the oils which leads to increased yields [70]. Sarmento et al. [82]
evaluated the effect of process temperature and pressure for the SFE of rice bran oil, enriched with
tocopherols and/or tocotrienols. The ranges of temperature and pressure studied were25–60 °C
and150–250 bar, respectively. Reduction in the density of the solvent was thought to be at the origin
of an increased in process yield increased with decreasing process temperature at constant pressure.
Diofanor et al. [83] also studied the effects of temperature and pressure on the SFE process of oils
from grape seeds and showed that higher yields (10.5%) were obtained at lower temperatures (313K)
and attributed the observation to the high solvent power of SC-CO2 because it has a higher density at
the lower temperature. Using three CO2 flow rates (1–5 g/min), operating at 30 MPa, 40 °C, and a
particle size of 0.40 mm, it was established that higher flow rates lead to higher oil extraction yield
(9.8% and 10.5% at 1and 5 g/min, respectively). In addition, oil yield increased with a reduction in
particle size (10.5%and 9.4% at 0.80 and 0.40mm, respectively) at 30 MPa, 313 K, and 5 g/min. Hu et
al. (2013) reported maximum extraction at 60–80 mesh size in combination with temperature (30 °C),
pressure (343.5 MPa), and CO2 flux (80 mL) for oil extraction from Cuminum cyminum seeds. During
extraction of oils from two tucuma species (Amazon tucumã (AT) and Parátucumã (PT) fruits) it was
observed that sometimes the material is not very accessible to the supercritical solvent thereby
lowering yield [84].
From the preceding analysis, it is observed that recent research on vegetable oil extractions has
been focused more on the assisted methods (microwave and ultrasound) and supercritical fluid
extraction compared to the conventional solvent and mechanical extraction methods. Oil extraction
efficiency and oil quality is a function of the oil bearing material and the extraction method used.

3. Methods of Optimization for Vegetable Oil Extraction

Most optimization methods entail the application of statistical software to optimize the control
variables (extraction time, sample weight, solvent volume, nature of solvent, seeds’ variability, and
particle size, etc.) that seek reduce cost and increase performance while at the same time minimizing
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deterioration of the quality of the product as much as possible [18,85]. With respect to oil extraction,
two main methods of process optimization can be identified in the literature: the traditional or
conventional optimization method in which a single variable is changed at a time instead of all
simultaneously, sometimes referred to as single parameter optimization and that in which a number
of variables can be varied simultaneously to take care of interactions that can occur between the
factors known as design of experiments (DOE) [86].

3.1. Single Parameter Optimization

To determine the best conditions for oil extraction some researchers have taken the approach of
changing a single factor at a time while other factors are kept constant [87]. In this case the ideal level
for one factor which provides the best response is defined. This process is not only laborious but
erroneous as it does not consider interactions because the optimum level of a factor is determined
based on certain levels of other factors. These optimum levels could change if different values of the
constant factors are considered [87]. The ability of this method to estimate interaction between
factors is limited by the demand of more experimental runs without changing its precision. Due to
these limitations of the one parameter optimization, this review is based principally on optimization
methods that allow the evaluation of the interaction effect of process variables on response factors
being studied.

3.2. Design of Experiments for Oil Extraction from Plant Seeds

3.2.1. Response Surface Methodology (RSM)

Response Surface Methodology (RSM) uses a number of mathematical and statistical
techniques which are employed to model and analyze problems in two or more process variables
that have an influence on the intended response [4,16,85,88,89] and the objective is to identify the
optimal operating conditions for a system under study [90,91]. RSM is based on relating product
properties to regression equations that describe inter-relations between input parameters and
product properties [26,92]. A major step in optimization is screening the factors studied in order to
have the significant effects of the analytical method [93]. RSM reduces the number of experimental
runs but maintains the expected accuracy and in addition determines responses for the interactive
effect of different variables [94]. The RSM is limited in that data is fitted to a polynomial at the
second level but all the systems with curvature might not be compatible with a second-order
polynomial model [87]. Amongst the many RSM designs available, the central composite design
(CCD) and the Box-Behnken design (BBD) have been popularly used for oil extraction processes.

Central Composite Design (CCD)

CCD is one of the most commonly used designs in oil extraction processes. Olaoye and Busari
[95] stated that this method is preferred when fitting a quadratic surface and it helps to optimize the
factors with reduced experimental runs while taking care of interaction between factors. Ogunleye et
al. [96] used a CCD with three independent variables (extraction temperature, compression force,
and mass of seed) at five levels to perform a total of 20 experiments including eight factorial, six
axial, and six center points to optimize mechanical extraction of castor oil from its seeds. The ranges
of the parameters studied were 40–200 °C, 550–750 kN, and 20–100 g for extraction temperature,
compression force, and mass of seed, respectively, while the response measured was the oil yield
(%). Optimum reaction conditions were 45 °C reaction temperature, 745.38 kN force, and mass of
99.88 g which gave an optimum crude oil yield of 31.01%. Hui et al. [97] used a CCD with two
variables each at five levels to optimize the UAE extraction of raspberry seed oil. The effects of
process variables, sonication time and extraction temperature on oil recovery and quality (vitamin E
content, and antioxidant capacity), were investigated. The fitted models gave significant p-values of
0.0007, 0.0035, and 0.0022 for extraction yield, vitamin E content, and antioxidant capacity,
respectively, with corresponding R2values of 0.93, 0.89, and 0.90. In addition, lack of fit for all the
three responses were insignificant with values greater than 0.05. The analysis of results from the
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microwave assisted extraction yield of sandalwood oil by Kusuma and Mahfud [28] (2016), using
CCD with the following independent variables: microwave power (400–800 W), plant material to
solvent ratio (0.10–0.20 g mL−1), and extraction time (C: 40–120 min) showed that the developed
polynomial represented the data very well with the R2 and R2adjvalues of 0.9594 and 0.9229,
respectively. Other forms of CCDs such as Central Composite Rotatable Designs (CCRD) and Faced
Centered Composite Design (FCCD) have also been reported in the literature for oil extraction
processes.

Central composite rotatable designs (CCRD)

The use of CCRD is also common and widely acceptable for multi-variable optimization [98].
For example, Bamgboye and Adejumo, [99] applied a five factor four level CCRD for the
optimization of the mechanical press extraction of oil from roselle oilseeds. The factors studied were
applied pressure, moisture content (% dry basis), heating temperature, heating time, and pressing
time for both fine and coarse samples. The R2 and standard error (SE) values obtained for the fine
and coarse samples used in the study were 0.98 and 1.53% and 0.97 and 1.64%, respectively, which
indicated a good fit for the experimental data. Olaoye and Busari [95] optimized the mechanical
expression of castor seed oil using CCRD. The effect of reaction temperature, reaction time, and
moisture content on oil yield was evaluated and a maximum yield of 26.5% was obtained at
moisture content, heating temperature, and reaction time of 6.68%, 100 °C, and 15 min, respectively.
The resulting R2 and R2Adj for the selected model were 0.9883 and 0.9778, respectively, which
demonstrated the suitability of the equation to fit the data obtained. The very low p-value of
moisture content (<0.0001) showed that it had the most significant effect on the process. Badwaik et
al. [100] also used the CCRD to evaluate the suitability of different solvents for the extraction of oil
from defatted peanut. Hexane was a preferred solvent compared to acetone, benzene, chloroform,
and petroleum ether under the reaction conditions of solvent/solute ratio and extraction time of 1:6
and 5 h, respectively, with an R2 value of 0.900 for the developed model. A three-factor five-level
CCRD was used by Jiyane et al. [101] to study Croton gratissimus seeds’ oil extraction. The effect of
extraction time, extraction temperature, and solvent-to-feed ratio on the oil yield was investigated
using n-hexane and ethyl acetate as extraction solvents. R2 of the models developed were 0.98 and
0.97 for n-hexane and ethyl acetate extraction, respectively, which demonstrated that the models
developed adequately represented the processes studied.

Faced Centered Composite Design (FCCD)

Another type of CCD that has also been employed in modeling oil extraction processes is the
Faced Centered Composite Design (FCCD). Erna et al. [3] optimized the mechanical oil extraction
from Jatropha curcas L. kernel using a FCCD in which the effects of applied pressure, temperature,
and moisture content of the oil seed on oil yield were studied. Contrary to Erna et al. [3], who
reported a moisture content of 7% required for optimum oil extraction, Olaoye and Busari [95]
reported a lower moisture content of 4% (w.b). The difference was attributed to the type of seed
material used. The R2 and R2Adj for oil extraction from Jatropha curcas L. kernel were 0.987 and 0.975,
respectively, which indicated that the estimated model fitted the experimental data satisfactorily. In
the SFE of sunflower oil, Amit et al. [102] used a FCCD to obtain R2, R2adj, and predicted R2 values of
0.9998, 0.9989, and 0.3848, respectively, for the selected quadratic model. The very low value for
predicted R2 was explained by the presence of many insignificant values in the model.

Box-Behnken design (BBD)

BBD does not include experimental runs for which the upper and lower limits of the factors are
simultaneously measured and therefore is not suitable for experiments performed at extreme
conditions [57]. This is however a limitation for experiments where the results for these extreme
cases are necessary. Faiznur et al. [16] used the BBD to optimize UAE of oil from Calophyllum
inophyllum by studying the effects of extraction time, ultrasound power, extraction temperature, and
Processes 2020, 8, 209 9 of 21

liquid to solid (L/S) ratio) on the oil yield. The experimental data was fitted to a quadratic model
using multiple regression analysis to obtain an R2 value of 0.984. The predicted oil yield was
optimum (56.2%) when the extraction was conducted for 21 min, 210 W ultrasound power, 42 °C
extraction temperature and 21 mL/g L/S ratio. These results were very close to the experimental
values, meaning that the BBD was successful in optimizing the extraction process. Using the BBD
Ogbeide et al. [103] studied the optimization of the extraction process conditions of gmelina seed oil.
The interaction effect of process parameters agitation time (10–60 min), volume of solvent (50–150
mL), and particle size (150–1000 μm) on oil yield was evaluated. The optimum conditions of seed
particle size of 150 μm, solvent volume of 150 mL, and agitation time of 60 min gave an oil yield of
52.09%.The BBD has also been used to optimize UAE processes. For example, Faiznur et al. [16] used
the BBD to optimize UAE of oil from Callophyllum inophyllum. Parameters optimized were extraction
time, ultrasound power, extraction temperature, and liquid to solid (L/S) ratio to obtain an optimum
yield of 56.2% when the extraction was conducted for 21 min, at 210 W ultrasound power at 42 °C
with a 21 mL/g L/S ratio. The selected model had an R2 value of 0.984. Oniya et al. [30] also used BBD
to optimize solvent extraction of oil from sandbox kernel. An optimum oil yield of63.4% was defined
under optimum conditions of seed/solvent ratio 0.05 g/mL, extraction temperature 68.13 °C, and
extraction time of 5 h.
Some few studies have been dedicated to the comparison of the designs commonly used in
optimizing oil extraction from oilseeds. For example, Olivera et al. [104] used the extraction of
hempseed oil (HSO) to compare BBD, FCCD, and Full Factorial Designs (FFD) basically to see if the
simple BBD and FCCD could replace the more complex and expensive FFD. All tested models were
significant with a confidence level of 95%. The R2 for BBD was 0.942 compared to that for FCCD,
which was 0.742, showing that the BBD had the best value. Even though their R2 values differed they
all gave the same optimal temperature. FFD models defined a lower solvent-to-seed ratio and a
slightly shorter extraction time than the BBD and FCCD-based models. All the models predicted best
HSO yields which were close to the experimental yields obtained under the same optimum
extraction conditions (about 30 g/100 g). In other fields the BBD and Doehlert have also been shown
to be better than the CCD, but much more efficient than the traditional FFD [104]. Table 1
summarizes some common plant material whose oil extraction conditions have been studied by
RSM.
Processes 2020, 8, 209 10 of 21

Table 1.Response Surface Methodology (RSM)parameters, type of oilseed, and solvent type on oil yield.
Optimum
Plant Material/Seed Used Parameters Studied Method Solvent/or Enzyme RSM Optimum Conditions References
Yield
Solvent
Extraction time, solvent volume, and Extraction time = 30.00 min, seed variability = 45.650%
Parts of Africa, extractio n-hexane BBD [18]
Neem powder weight 181.896 mL, and Neem powder weight = 30 g (w/w)
Neem seeds Indian n
subcontinent Extraction time, temperature, Extraction time 24 min, temperature 80 °C,
MAE n-hexane Doehlert 31.68% [65]
solvent/solute ratio solvent/solute ratio 3:1
Central and West Extraction time, temperature, Extraction time 24 min, temperature 80 °C,
Sheanut kernels MAE n-hexane Doehlert 31.58% [69]
Africa solvent/solute ratio solvent/solute ratio 3:1
Mexico and
Type of solvents,temperature, solvent 8 h reaction time, temperature of around 68 °C,
central America, Petroleum ether Not
Jatropha curcas to solid ratio, processing time, and CSE coarseparticle size (0.5–0.75 mm), solvent to solid [105]
lately parts of n-hexane applicable
particle size of the meal ratio of 6:1, and hexane as solvent
Tropical Africa
Tropical America Extraction time 4.5 h, extraction temperature 65 °C,
Polarity, extraction time, and extraction Petroleum ether Not 51.88%±3.1
Thevetia peruviana and Tropical CSE petroleum ether to methanol ratio 90:10 (polarity [106]
temperature Methanol applicable 8%
Africa index 0.6)
Mainly Japan,
Thailand, India, Temperature, stirring rate, solvent-bran Temperature 55 °C, solvent-bran ratio 6:1, stirring
Rice bran CSE Acetone, ethanol CCD 82% [107]
China, and ratio, and contact time rate 180 rpm, and contact time45 min
Vietnam
Raw material size, raw material to
Ocimum basilicum India, Africa, and Water-to-material ratio of 3.2:1,extraction time of 97
water ratio, extraction time, and MAE Water CCD 0.6% [108]
L. South East Asia min, and microwave power of 430 W
microwave power
Roasting temperature (87.70–172.0 °C)
Gourd seeds ME Not applicable CCRD Roasting temperature 100 °C, roasting time 20 min 27.62% [109]
Canada, and roasting duration (7.93–22.07 min)
Argentina, South Microwave power (110–1100 W),
Elateriospermumta and Central extraction time (30–120 s), enzyme Cellulase pectinase 110 W microwave power, 30 s extraction time, 1 % 46.12% ±
MAE CCD [39]
pos seed America cocktail concentration (1%–5%), and proteinase cocktail enzyme, and0.5 mm particle size. 1.48 %
particle size (0.5–1.5 mm)
South China,
Thaïlande,Laos,M Enzyme ratio/% (5–25), reaction
Pectinase, protease, Enzyme mass per volume ratio of 14.6%, incubation
Momordicacochin yanmar, time/min (60–180), reaction
EAE a-amylase and CCD time of127 min, temperature of 58 °C, and stirring 79.5% [110]
chinensis(Gac fruit) Cambodia,Vietna temperature/°C(40–80), stirring
cellulose speed of 162 rpm
m,North East speed/rpm (50–250)
Australia
Solvent to seeds ratio, reaction time, Solvent to seeds ratio 14:1, reaction time 4.4 h, and
Jatropha seed CSE n-hexane BBD 51% [111]
and reaction temperature reaction temperature 35 °C.
Amazon forest of Water, cellulase,
Temperature, enzyme concentration, Temperature 55 °C, 2% enzyme concentration, and
Mauritia Flexuosa Brazil and Peru, EAE pectinase, and CCRD 76.5% [112]
extraction time 6 h extraction time
South America protease
Citrus sinensis Tropics Roasting time, roasting temperature CSE NA CCRD Roasting temperature170 °C, roasting time 30 min 56%±6.5% [91]
Croton gratissimus Tropical and Seed to solvent ratio, extraction time, CSE ethyl acetate CCRD Seed to solvent ratio 5 mL/g, extraction 9.21% [101]
Processes 2020, 8, 209 11 of 21

Sub-Tropical extraction temperature n-hexane, temperature: 35 °C (both solvents) extraction time6

Africa min with n-hexane, 20 min with ethyl acetate
Tropical and Extraction time, ultrasound power,
Calophylluminophyll Extraction time 21 min, ultrasound power 210 W,
some temperate extraction temperature, and liquid to UAE n-hexane BBD 56.2% [16]
um extraction temperature 42 °C, and L/S ratio 21 mL/g
regions solid (L/S) ratio
Middle
East,Caucasus
Power (176–300 W), time (5–20 min),
region, North and Microwave power of 220 W, particle size in the
particle size (d=0.125–0.800 mm), and
Pomegranate seed TropicalAfrica, MAE n-hexane FCCD range of d=0.125–0.450 mm, and solvent-to-sample 35.19% [61]
solvent to sample ratio (2:1, 6:1, and
the Indian ratio of 10:1 (by mass) in 5 min extraction time
10:1, by mass)
subcontinent,
Central Asia
Pomegranate(Punic Pressure, temperature, extraction time, 350 atm pressure, 55 °C temperature, 30 min
SFE Methanol CCD [73]
agranatum L.) peel and modifier (methanol) volume extraction time, and 150 µ L methanol
Sonication time and extraction Sonication time of 37 min and extraction
Raspberry seed oil Temperate zones UAE Not mentioned CCD 23% [98]
temperature temperature of 54 °C
Processes 2020, 8, 209 12 of 21

4. Modeling and Validation of Models

In RSM, the phenomenon being studied is usually represented by Equation (1)

Y = f (Uij) (1)

Y is the dependent variable of interest to be measured usually referred to as the response. Uij are
the independent variables that can influence a particular response normally called factors. f is a
mathematical function which predicts the different responses depending on the values of Uij. A
second order polynomial with interaction (Equation (2)) is widely used to model the responses
[18,71,101,102].

𝑘 𝑘
(2)
𝑌 = 𝑏0 + ∑ 𝑏𝑗 𝑥𝑗 + ∑ 𝑏𝑗𝑗 𝑥𝑗2 + ∑ ∑ 𝑏𝑖𝑗 𝑥𝑖𝑗
𝑗−1 𝑗−1 𝑖<𝑗

whereb0, bi, bjj, and bij are regression coefficients for intercept, linear, quadratic, and interaction terms,
respectively, and xi and xj are coded independent variables. Many extraction processes used the
regression coefficient R2 and/or absolute/standard error of deviation (SED) for the validation of the
models used. A model is considered good if R2> 0.70 and/or SED < 10% [113].

5. Types of Software Used

The use of response surface methodology in food science has increased in recent years
[36,42,62]. During optimization a second order polynomial is developed to model the responses and
data obtained from optimization is sometimes subjected to simple ANOVA, t-test [36], and/or to
some free or commercial statistical packages (Table 2). Design Experts (Stat-Ease, Inc., Minneapolis,
MN, USA) was used to optimize the microwave extraction of pomegranate seed oil, mechanical
extraction of gourd seed oil [58,108], Sigma plot version 12.5for CSE of oil from neem seed [66].
Paramita et al. [114] used MATLAB Version 5.0 to analyze data from the supercritical carbon
extraction of cotton seed oil. IBM SPSS was the statistical package chosen by Krunoslav et al. [115]
(201) in their work on the supercritical carbon extraction of hemp seed oil. Minitab version 15.5 is
also commonly used [116].
 Processes 2020, 8, 209 13 of 21

Table 2. Summary of model validation parameters and type of modelling software use.
Plant Parameter (s) Model Validation
DOE Used DP Used Value of R2 SED etc. Quality Parameters Quality Value Validity Software used References
Species Analyzed Criteria Used

Neem Oil yield R2 SED Valid

Doehlert 2 R2and SED Oil yield: 0.862 Oil yield: 2.45% Acid value 4.02 mg of KOH/g oil Sigmaplot 12 [65]
seeds Acid value Valid
Acid value: 0.884 Acid value: 5.40%
Design
Yield: 0.79, Expert Version
Ofada RSM (Specific Yield, free fatty Moisture content 43.00%±1.41% w.b
Fatty acids: 0.91, 8.0.1.0
rice type not acid, color, and 2 R2 Acid value 8.13%±0.78% Valid [117]
Color: 0.99, and (StateaseIn;
brand mentioned) peroxide value Refractive Index 1.461±0.01
Peroxide value: 0.99 Minneapolis
USA, version).
Iodine value 112.31mg of I2/100g
Neem Box-Behnken Saponification value 198 mg of KOH/g Design Expert
Yield 2 R2 Yield: 97.55% Valid [18]
seeds design FFA 1.91% 9.0.3.1
Acid value 3.82mg of KOH/g
“Design expert”
PistaciaK Central
(version 5) and
hinjuk composite Yield 2 R2 Yield: 0.99 Valid [30]
“Statistica”
Seeds design
(version 5)

R2 p-Value
Yield Yield: 0.83 Yield: 0.014
FFA FFA: 0.67 FFA: 0.001 Design Expert
FFA 1.4%
Central Refractive Refractive index: Refractive index: Version 6.0.10
Orange Color 4.7 abs
Rotatable index 2 R2and p-Values 0.80 0.24 All valid (Stat Ease [4]
seeds Specific gravity 0.92
Design Color Color: 0.91 Color: 0.002 Minneapolis,
pH 5.4
pH pH: 0.77 pH: 0.3 USA)
Specific gravity Specific gravity: Specific gravity:
0.91 0.001
R2
F-Value
Oil recovery:
Oil recovery:
Oil recovery 0.900
32.59
Surface Surface
Central Surface
appearance appearance: 0.822 “Design expert”
Peanut Rotatable 2 R2and F-Values appearance: 6.48 / / All valid [100]
Sensory color Sensory color: (version 5)
Design Sensory color:
Overall 0.800
4.60
acceptability Overall
Overall
acceptability:
acceptability: 7.38
0.845
Calophyll Design Expert
Box-Benkhen
uminophy Yield 2 R2 Yield: 0.984 -/ / Valid (Version 6.0.6, [16]
Design
llum Stat-
 Processes 2020, 8, 209 14 of 21

Ease Inc.,
Minneapolis,
Minnesota,
USA).
Acid value 1.8048 mg KOH/g oil
Concentration
Cannabis Concentration of tocopherols FFA 0.9024%
of tocopherols,
sativa L. 2 R2 Fatty acids Iodine value 97.60 g I2/100g oil Valid IBM SPSS [115]
fatty acids, and
seed Pigments Saponification value 57.5025 mg KOH/g oil
pigments
Cetane number 140.998
DP = Degree of polynomial, DOE = Design of experiment.
Processes 2020, 8, 209 15 of 21

6. Quality of Oil
In most studies, even though the quantity of oil obtained is the most studied response, some
researchers have also studied the effect of various parameters on the quality of the extracted oil. Free
fatty acid, saponification value, refractive index, moisture content, and color are some of the
responses that have been studied. The variables studied and the methods used have an effect on the
quality of the oil obtained. Following mechanical extraction and optimization of oils from gourd
seeds, Yetunde et al. [109] reported saponification value, refractive index, specific gravity, FFA, and
color of 289.66 mL, 1.47, 0.90 g/mL, 0.61%, and 3.47 abs, respectively. Nde Bup et al. [118] reported
optimum ranges of 5–20 min cooking time and 40–50 °C cooking temperature for the extraction of
neem oil and indicated that the parameters analyzed (moisture content, refractive index, quantity of
oil, and acid value)were significantly affected by the independent factors. Optimum responses
obtained at the mid points of the optimum ranges for moisture content, oil content, acid value, and
refractive index were 46.37%w.b., 21.43%, 3.53 mg KOH/g oil, and 1.460, respectively. Under
optimum processing conditions of 19 MPa applied pressure, 90 °C pressing temperature, and 3.8%
(w.b.) moisture content, Erna et al. [3] obtained oil that met the DIN 51605:2010–10 standard for
fuels made from plant oils except for its phosphorus content and group II metals. Dang and Nguyen
[119] studied the effect of cold-pressing, solvent extraction, and enzyme assisted aqueous extraction
on the quality of oil extracted from cashew nuts. These methods were compared for oil quality
indicators, such as specific gravity, free fatty acid (FFA), peroxide values (PV), total phenolic (TPC),
total flavonoid content (TFC), fatty acid composition, and storage stability. Solvent extraction gave
higher yields but oil from cold-pressing was most stable against oxidization and rancidity and could
be kept fresh for 12 months, while the enzyme and solvent extraction oils lasted 8 months without
major changes, at room temperature. The work of Gutte et al. [53] on the ultrasonic extraction and
fatty acid profile showed 11.5% improvement of extraction yield at the optimum conditions of
frequency of 40 kHz, temperature of 30 °C, extraction time of 40 min, and solid to solvent ratio: 1:10.
They also reported an improved extraction of all fatty acids and a significant increase in
polyunsaturated fatty acids. Uitterhaegen et al. [120] reported that the screw configuration and
pressing temperature optimized in the screw press method of extraction had no significant effect on
the quality of the oil obtained. Pomegranate seed oil extracted by MAE showed a significantly
lower peroxide value (0 mmol of O2 per kg of oil), free fatty acidity (0.42%), and higher total phenolic
(7.42 mg/g) and antioxidant activity (5 mg/mL) compared to the cold extraction which gave 4 mmol
of O2 per kg peroxide value, 1.73 mg/g phenolic content, and an antioxidant activity of 17.00 mg/mL
[61]. The difference in antioxidant activity was attributed to differences in total phenolic content.

7. Conclusions
Oil extraction methods from oil seeds include conventional methods (solvent and mechanical
extraction) and nonconventional or improved techniques (supercritical fluid extraction, ultrasound,
microwave, and enzyme assisted extraction. These nonconventional techniques are innovative and
have potential to improve oil extraction rates, shorten extraction times, and minimize deterioration
of the oil quality. The nonconventional methods have been used successfully to reduce some of the
loopholes of the conventional methods of oil extraction. Response surface methodology is the most
commonly used method to optimize oil extraction from plant material. Box-Behnken and Doehlert
are better than the Centre Composite Design but much more efficient than the traditional full
factorial design. Design expert, Sigma Plot version 12.5, MATLAB version 5.0, IBM SPSS, and
Minitab version 15.5 have been commonly used to optimize the extraction of oil seeds. The variables
studied and the methods of extraction used have an effect on the quality of oil obtained. Some of the
quality parameters studied were saponification value, refractive index, specific gravity, moisture
content, FFA, and color. The majority of studies carried out on the nonconventional methods of oil
extraction have been centered on laboratory batch processes. There is need to extend the research to
continuous microwave and ultrasound assisted extraction as well as supercritical fluid extraction
systems at the laboratory scale and subsequent scale-up to both pilot and industrial systems. An
Processes 2020, 8, 209 16 of 21

important and useful extension of this work is to carry out the economic evaluation of the various
nonconventional extraction systems to evaluate their profitability.
Author Contributions: Divine Bup Nde conceived the topic and structure as well as corrected the manuscript.
Anuanwen Claris Foncha wrote the first draft of the manuscript. All authors have read and agreed to the
published version of the manuscript.

Funding: This research received no external funding.

Conflicts of Interest: The authors declare no conflict of interest.

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