Trends in Food Science & Technology 133 (2023) 99–113

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Trends in Food Science & Technology

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

Aqueous extraction processing: An innovative and sustainable approach for

recovery of unconventional oils
Guilherme Dallarmi Sorita a, b, Simone Palma Favaro b, Alan Ambrosi a, Marco Di Luccio a, *
a
Laboratory of Membrane Processes (LABSEM), Department of Chemical and Food Engineering, Federal University of Santa Catarina (UFSC), Trindade, 88040-900,
Florianópolis, Santa Catarina, Brazil
b
Empresa Brasileira de Pesquisa Agropecuária, Embrapa, PqEB, W3 Norte - Asa Norte, Brasília, DF, Brazil

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

Handling Editor: Dr I Oey Background: Unconventional crops (e.g., tiger nut, macaw, babassu, sesame, and others) are promising edible oil
sources. However, the traditional oil extraction methods, mechanical pressing, and solvent extraction show low
Keywords: efficiency or use environmentally unfriendly solvents (hexane). Aqueous extraction processing (AEP) has
Aqueous oil extraction recently emerged as a significant opportunity for achieving the sustainable development goal (SDG) to produce
Emulsion break
edible oils. This technology usually requires a pre-treatment step, e. g., milling, followed by a demulsification
Physical demulsification
step, which traditionally involves enzyme addition for free oil recovery. Optimizing the demulsification methods
Filter-coalescers
Membrane separation can lead to high oil yields (>95%), which is comparable to the use of hexane.
Biorefinery Scope and approach: This review discusses the scientific data and trends related to demulsification steps on AEP
for oil recovery, focusing on unconventional oil crops. New physical demulsification possibilities, such as filter
coalescers and membrane technology, are outlined as alternatives to traditional demulsification methods, which
present some drawbacks regarding process scalability and oil quality. Additionally, a complete route, with a
biorefinery approach, is suggested for the industrial application of oil and high-added-value compounds from the
by-products of AEP (liquid and solid fractions) as an opportunity to update the traditional oil production sector.
Key findings and conclusions: With the increased demand for conventional oils for biofuel purposes, exploring
unconventional crops is a viable and suitable alternative to obtain food-grade oil. Integrating AEP with physical
demulsification methods is an eco-friendly and promising strategy for producing high-quality oil from uncon­
ventional and minor crop sources since water is used as the solvent instead of hexane. Moreover, applying
biorefinery concepts is an opportunity to stimulate the circular economy and produce valuable compounds
(proteins, carbohydrates, fibers, and others) with beneficial health properties and wide application in food
industries.

1. Introduction
The world population will significantly increase in the next few
years; therefore, the pressure on natural resources to respond to food
needs is also growing, leading to global challenges regarding affordable
food supply and sustainability (Caldeira et al., 2020). The dietary de­
mand for edible oils has increased by 44% in the last decade with the
rapid expansion of the world’s population and economy (Altendorf
et al., 2019; Zhang et al., 2019). Thus, the challenges correlated to food
safety and production have been proportionally expanding. Moreover,
conventional oil crops have been extensively used for biofuel production
(Rodrigues et al., 2017), competing with food uses and affecting market
prices.
Alternative edible vegetable oils have drawn attention due to several
factors, for instance, increased awareness of health problems related to
trans fatty acids, increasing use of vegetable oil for biofuel feedstock
supply as an alternative for fossil fuels, and rising international concerns
over the environmental impacts of deforestation through palm logging
and conversion of rainforest to cropland for soybean production
(Rodrigues et al., 2017). Therefore, extensive research is required to find
new sustainable oil sources and extraction processes.
Unconventional edible oil sources or minor crops, such as tiger nut
(Hu et al., 2020), camelina seeds (Anderson et al., 2019), macaw
mesocarp and kernel (Lieb et al., 2019; Vargas-Carpintero et al., 2021),

* Corresponding author.
E-mail address: di.luccio@ufsc.br (M. Di Luccio).

https://doi.org/10.1016/j.tifs.2023.01.019
Received 2 May 2022; Received in revised form 16 January 2023; Accepted 27 January 2023
Available online 30 January 2023
0924-2244/© 2023 Elsevier Ltd. All rights reserved.
G.D. Sorita et al.
cardoon (Mandim et al., 2020), babassu fruits (Santos et al., 2020) and
others emerge as alternatives to traditional oil sources. A considerable
oil recovery (23.1–85.2%) can be obtained from these unexplored or
underexplored sources, which are economically viable for human con­
sumption (frying and salad oils, mayonnaise, confectionery fats, ice
cream, functional foods, and others).
Mechanical (expellers) and solvent extraction are the most used
processes for edible oil extraction. In the mechanical method (also called
cold pressing extraction), the raw material is placed between two bar­
riers where the volume available to the raw material is reduced by
pressing and expelling the oil. This well-established method has a low
yield because the oil is physically forced out of the vegetable matrix,
leaving a cake (by-product) with significant oil content (15–20%). In
this method, a subsequent step is necessary for better oil yield, in which
the cake is submitted to solvent extraction (Yang, Wen, et al., 2021).
The solvent extraction typically uses hexane due to its high oil sol­
ubility, leading to a high oil yield and easy recovery. Solvent extraction
is more efficient than mechanical pressing because solvent (in this case,
hexane) can penetrate the raw material through the vegetable matrix
pores and walls and solubilizes the oil. Nevertheless, organic solvents
are environmentally unfriendly, flammable, and can evaporate, causing
dizziness, nausea, and headache to operators (Nde & Foncha, 2020;
Punia et al., 2021). Post-treatment steps for solvent removal and oil
refining (degumming, neutralization, bleaching, and deodorization) are
required. Extensive research has been undertaken to find alternative
extraction methods for industrial oil recovery, focusing on quality, high
extraction yield, and using environmentally friendly solvents to replace
hexane.
Aqueous extraction processing (AEP) emerges as a friendly alterna­
tive since it offers advantages like eliminating organic solvent con­
sumption and requiring lower investment costs and energy demand.
Additionally, AEP does not require equipment for drying, solvent re­
covery, and volatile organic compounds (VOCs) emission monitoring
and control. In addition, this process enables the simultaneous recovery
of other compounds, such as proteins, carbohydrates, and fibers (Cater
et al., 1974; Geng et al., 2020; Li et al., 2014; Rosenthal et al., 1996).
AEP has been applied to unconventional edible oil sources such as
moringa seeds (Yusoff et al., 2016), sesame seeds (Tirgarian et al.,
2019), and castor seeds (Díaz-suárez et al., 2021). Despite the potential,
earlier AEP studies showed low oil yield (~60%) due to the formation of
a stable cream emulsion (formed by oil, water, and emulsifiers naturally
present in the vegetable matrix: proteins, carbohydrates, fibers, and
phospholipids from the milling raw material). The total destabilization
of the cream to release the oil is required to improve the oil recovery,
which is a relevant challenge to the commercial viability of any aqueous
extraction procedure (Liu et al., 2020; Souza et al., 2020). A robust
demulsification method can lead to higher yields and renew the op­
portunities of this value chain.
Recently published studies are focused on biological, chemical, and
thermal demulsification (Liu et al., 2020; Xu et al., 2021; Yusoff et al.,
2015). However, to date no study has addressed the physical demulsi­
fication (such as the use of coalescers and membranes) on AEP for oil
recovery and vegetable oil demulsification. Since physical demulsifica­
tion has been successfully applied in separating oil and water in
wastewater treatment and petroleum industries (Abed et al., 2019;
Ajogbeje et al., 2021; Guan et al., 2021), those processes could be
adapted to AEP processing, improving the oil recovery. Additionally,
several studies suggest the possibility of using solid by-products to
produce functional ingredients due to their high content of valuable
compounds, including protein, polysaccharides, fibers, and other com­
pounds (Harith et al., 2019; Li, Sun, et al., 2020; Sánchez-Zapata et al.,
2010; Sorita et al., 2020). In this context, an efficient AEP optimized for
various oil sources can produce numerous distinct products and conse­
quently promote valorization strategies based on sustainable technolo­
gies endorsed in a biorefinery concept, which is the framework where
renewable raw materials and their residues (biomass) are transformed
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Trends in Food Science & Technology 133 (2023) 99–113
into food and high added-value products, with a lower generation of
waste and pollutants (Bonan et al., 2022).
This review aims to discuss the current state of the art of new un­
conventional oil sources, focusing on the successful possibility of AEP
application for industrial edible oil recovery. The review also assesses
the application of physical demulsification as an alternative to con­
ventional demulsification methods (biological, chemical, and thermal).
The use of the AEP by-products as promising food ingredients was also
compiled in this review, suggesting a process upgrade through the bio­
refinery concept (combining physical demulsification methods and
obtaining several products, such as pectin, phospholipids, carbohy­
drates, proteins, and fibers).
2. Unconventional and minor vegetable oil sources and their
benefits for edible oil production
Diversifying oilseed sources is essential for all countries to meet the
growing demand and guarantee less dependence on imports. The so-
called unconventional oil sources, here referred as the sources that are
not part of the traditional commodities, are being used to supply the
demand and keep in line with sustainability criteria. Edible oils and fats
can come from by-products or minor and neglected crops and insects
(Mariod et al., 2017; Tzompa-Sosa et al., 2019). It is worth pointing out
that the term conventional or unconventional also relies on cultural
aspects beyond their share in the global market. For instance, cottonseed
oil is considered a conventional vegetable oil in many countries except
India (Choudhary et al., 2014). Several reports describe the oil recovery
(23.1–85.2%) from unconventional sources such as tiger nut (Hu et al.,
2020), macaw kernel and pulp (Lieb et al., 2019), babassu fruits (Santos
et al., 2020), sesame (Morris et al., 2021) and others. The diversity of
vegetable oil sources with potential uses for edible oil production, such
as the oil content and the fatty acid composition, is presented in Table 1.
The high demand for food-grade oil and the competition with the bio­
fuels industry motivate food industries to exploit plants with significant
oil content and yield (up to 85.2% recovery was reported in the litera­
ture) and green and environmentally friendly extraction strategies.
There are numerous species of promising vegetables for oil produc­
tion. Buritirana, the Macaw palm fruit, and other palm fruits have
attracted scientific interest because they achieve high oil yields and are
good sources of bioactive compounds (Souza et al., 2021; Var­
gas-Carpintero et al., 2021). Buritirana (Mauritiella armata Mart.), a
Brazilian fruit species (Amazon and Cerrado region) belonging to the
Arecaceae family, has high nutritional and functional potential yet is
little explored. A study by Souza et al. (2021) shows that Buritirana
fruits comprise 41.57% of oil (mainly composed of oleic acid) with
antioxidant potential. Twenty bioactive compounds were identified in
the oil fraction by ESI-LTQ-XL-MS/MS, such as five organic acids, seven
phenolic acids, and eight flavonoids that can be used in food, cosmetic
and pharmaceutical industries. The buriti (fruit from Buritirana) pulp is
currently consumed in several ways (e.g., as raw fruit, juices, candies,
ice cream, wines, and fermented beverages). However, policies to
encourage cultivation, production, and commercial uses should be
adopted.
Macaw (Acrocomia spp) is another example of high oil content fruit
and yield per area, found in Brazil, spread in the Southeastern and
Central regions and other countries of Tropical America (Cardoso et al.,
2017; Vargas-Carpintero et al., 2021). Studies performed by Oliveira
et al. (2021) show that the oil content of macaw mesocarp ranged from
29.5 to 74.5% in 630 fruits collected in Minas Gerais State. Mono­
saturated fatty acids represent about 71.5% of total oil (with oleic acid
representing 70% of total oil), while polyunsaturated fatty acids corre­
spond to only 2.6%. Around 19.22% of total fatty acids are composed of
saturated fatty acids, being 17% (of the total oil content) of palmitic acid
(C16:0). It is important to note that the range in oil content and
composition are related to the plants’ genetic variability, maturity, and
growing region. Genetic breeding and complete domestication will
G.D. Sorita et al. Trends in Food Science & Technology 133 (2023) 99–113

Table 1
Unconventional vegetable oil sources with potential uses for edible oil production.
a
Unconventional sources Oil yield Extraction/ Fatty acids composition of the oil References
quantification method

Tiger nut (Cyperus
esculentus L.)
Camelina (Camelina sativa)
seeds
Macaw (Acrocomia
aculeata) mesocarp and
kernel
Buritirana (Mauritiella
armata Mart.) pulp
Cardoon (Cynara
cardunculus L.)
Babassu (Attalea speciosa)
fruits
Pennycress (Thlaspi
arvense)
Sesame (Sesamum indicum)
Pistacho (Pistacia vera L.)
kernel
Pequi (Caryocar brasiliensis
Camb.) fruits
Macadamia (Macadamia
integrifolia) nuts
Avocado (Persea americana
Mill.) pulp
a
[mass of extracted oil (g)/mass of dry raw material(g)] * 100.
29.9% Soxhlet Palmitic, palmitoleic, cydonic, stearic, oleic, α-linolenic, arachidic, and Hu et al. (2020)
eicosenoic acids
32.3% Soxhlet Palmitic, stearic, oleic, linoleic, linolenic, arachidic, eicosenoic, Anderson et al. (2019)
eicosadienoic, arachidonic, behenic, erucic, docosahexaenoic, and
nervonic acid s
Kernel: 56.1% Soxhlet Caprylic, capric, lauric, myristic, palmitic, palmitoleic, stearic, oleic, Lieb et al. (2019)
Mesocarp: 23.4% vaccenic, linoleic, and α-linolenic acids
41.6% Supercritical Palmitic, stearic, oleic, oleic, and linolenic acids Souza et al. (2021)
23.1% Soxhlet Caproic, caprylic, capric, lauric, myristic, pentadecanoic, palmitic, Mandim et al. (2020)
palmitoleic, heptadecanoic, stearic, oleic, linoleic, arachidic, gadoleic,
eicosadienoic, behenic, eicosenoic, eicosapentaenoic, tricosanoic, and
lignoceric acids
34.0% Mechanical pressing Caprylic, capric, lauric, myristic, palmitic, oleic, linoleic, and stearic Santos et al. (2020)
acids
28.7% Pulse nuclear magnetic Nervonic, palmitic, stearic, oleic, linoleic, linolenic, eicosenoic, Altendorf et al. (2019)
resonance (pNMR) eicosadienoic, erucic, and docosadienoic acids
47.3% Nuclear magnetic Palmitoleic, heptadecanoic, margaric, α-linolenic, eicosanoic, Morris et al. (2021)
resonance (NMR) eicosenoic, behenic, lignoceric, palmitic, stearic, oleic, and linoleic
acids
58.5% Maceration Palmitic, palmitoleic, stearic, oleic, linoleic and linolenic acids Yahyavi et al. (2020)
46.5% Soxhlet Myristic, palmitic, palmitoleic, stearic, oleic, linoleic and linolenic Cornelio-Santiago
acids et al. (2022)
74.16% Maceration Myristic, palmitic, palmitoleic, stearic, oleic, linoleic, linolenic, Shuai et al. (2022)
arachidic, gondoic, behenic, erucic and lignoceric acids
62.66% Soxhlet Palmitic, palmitoleic, stearic, oleic, linoleic and linolenic acids Tan et al. (2017)

increase productivity of this promising species.
Another unconventional oil source is Moringa oleifera kernels. This
source is native to the sub-Himalayan region and found in Northern
India, the Middle East, and African and Asian countries. The kernels
contain approximately 40% of oil (more than 70% is oleic acid), 31.4%
protein, 18.4 carbohydrates, 7.3% fiber, and many nutrients (such as
β-carotene, antioxidants, and minerals). They can be a substitute for
olive oil due to the similar monounsaturated fatty acid content. Moringa
oil has bioactive compounds (alkaloids, flavonoids, phenolic acids, and
tocopherols) with many reported human health benefits and may act to
reduce cardiovascular diseases, strokes, ulcers, joint pain, and stom­
achache, as reported in vitro and in vivo studies (Leone et al., 2016).
Cultivated in tropical and sub-tropical areas, sesame (Sesamum
indicum L.) seeds also emerge as a potential high yield (29.43–54.69%)
and quality oil (Morris et al., 2021). Besides the rich unsaturated fatty
acids (palmitoleic, oleic, linoleic, linolenic, and gadoleic acids), this seed
contains several bioactive compounds (protein, lignans, tocopherol, and
others). In addition, its consumption is related to several health benefits,
including high antioxidant activity, obesity prevention, and protection
against metabolism disorder (Dossou et al., 2022). They are also effec­
tively used in traditional medicine for inflammation, toothache, burns,
headaches, ulcers, and others (Morris et al., 2021).
Pistachio (Pistacia vera L.), a peculiar organoleptic nut, is another
unconventional oil source in food manufacturing. This nut is widely
consumed raw or toasted and salted and used as a food ingredient
worldwide. Pistachio kernel presents a high oil yield (49.9–58.5%) with
considerable amounts of oleic, linoleic, and linolenic acids, which are
linked to several health benefits, as mentioned previously. Additionally,
this source is rich in bioactive and health-promoting compounds that
can be extracted with the oil, such as tocopherols, sterols, and phenolic
compounds (Yahyavi et al., 2020), enhancing oil oxidative stability.
Therefore, AEP emerges as an innovative process for oil and other
valuable compounds (proteins, carbohydrates, fibers, and others) for
those interesting underused raw materials. In this sense, government
engagement for the diversification of crops for oil production allied with
biometric and agricultural aspects, genetic studies, green extraction
techniques, and biorefinery approaches may be a viable upgrade for oil
industries.
3. Aqueous extraction process (AEP)
The extraction process is the foremost step for oil recovery and for
producing new ingredients from raw materials (Mitra & Mishra, 2019).
Besides, the optimization steps of the extraction parameters are also
crucial for an efficient oil recovery process (Molino et al., 2020). In
addition, the process optimization depends on (i) the oil deposition in
the vegetable parts (kernel, seed, or pulp), (ii) the physical-chemical
properties of the oil, and (iii) possible applications (pharmaceutical,
cosmetic, or food industry). Moreover, AEP procedures must be robust
enough to ensure oil quality following current laws and regulations
(volatile compounds, insoluble impurities, soap content, iron, copper,
acidity, and peroxide value).
Maximizing oil yields and minimizing oil degradation and alterations
in the quality of the product is the key to extraction techniques (Kumar
et al., 2017). The recovery process must be as green and sustainable as
possible, with minimal waste generation, fitting to Green Chemistry
principles (Herrero & Ibañez, 2018). Those attributes are achieved when
AEP is used to produce edible oil. This section discusses the advantages
and drawbacks, the extraction mechanism, the oil body structure and its
influence on emulsion formation, and the very stable emulsion systems
formed in AEP.
3.1. Advantages and drawbacks of AEP
As Rosenthal et al. (1996) reported, AEP has numerous advantages,
such as being environmentally clean and safer since the emission of
flammable and volatile organic compounds is eliminated. This process
can produce edible oil, protein, and other valuable compounds.
Furthermore, the proteins’ structure is well preserved, contributing to
their functional properties as a food ingredient, adding value to this

101
G.D. Sorita et al.
co-product. Regarding cost-effectiveness, AEP could be worthy because
there is no need for some unit operations, such as desolventization. The
AEP-extracted oil has better quality (in terms of physicochemical pa­
rameters) than the press or solvent-extracted oils and could be directly
used as edible oil without refining (Tirgarian et al., 2019). Another
critical aspect of the AEP is processing high moisture content raw ma­
terials, with no need for drying to be feasible for hexane or pressing
extractions. Thus, since no drying pre-step is required, less energy is
demanded by employing an aqueous process.
Cheng et al. (2018) compared the environmental impact of AEP of
soybean oil with mechanical pressing and solvent extraction, using mass
flows, energy consumption, and the global warming potential of each
process. The three processes are similar in the vegetable matrix pre­
treatment steps (cleaning, cracking, hull removal, conditioning, and
flaking), and those steps can directly influence energy consumption. For
example, solvent extraction requires comminution of the raw material to
improve solvent diffusion inside the matrix, leading to higher energy
consumption. In the mechanical pressing route, the extrusion and
pressing are also energy intensive. Of these three processes, solvent
extraction has the highest power consumption since desolventization is
a critical step to remove residual hexane from the oil and by-products
(meal). On the other hand, AEP was considered a greener process due
to lower environmental impacts and reduced total energy consumption
compared with hexane extraction, leading to lower greenhouse gas
(GHG) emissions than mechanical pressing.
There could be some constraints of AEP in large-scale applications:
(i) low efficiency in free oil content, (ii) demulsification to separate the
oil, and (iii) treatment of the resulting aqueous waste (Rosenthal et al.,
1996). It is worth mentioning that non-fat compounds are simulta­
neously extracted with the oil, and the oil purity may decrease. The
importance of those issues depends on the raw material characteristics
and the availability of suitable processing machinery. Alternatives to
overcome those hurdles are addressed in this review.
3.2. Extraction mechanism
AEP is an environmentally friendly processing method that can also
be used for oil, protein, and phospholipid simultaneous extraction from
different biomasses and may be a viable alternative to hexane oil
extraction. The AEP mechanism is based on the insolubility of the oil
within the water. The emulsions formed during AEP have three main
constituents: (i) oil, (ii) water, and (iii) emulsifiers. The water solubilizes
the compounds that act as emulsifiers (vegetable cell components:
phospholipids, proteins, carbohydrates, and others) instead of the oil,
facilitating the oil-water and water-soluble compounds separation
(Díaz-Suárez et al., 2021). The traditional process mainly includes a
mechanical pre-treatment for grinding the plant tissue structures,
extraction, and physical treatments (e.g., centrifugation) for product
separation (Favaro et al., 2022). After centrifugation, AEP generates
four fractions: (i) free oil, (ii) cream (oil-rich fraction), (iii) solid
by-products (protein/fiber-rich fraction), and (iv) aqueous fraction
(soluble proteins and sugars and minor compounds). The proportions of
each fraction can vary according to the raw material and with extraction
parameters (such as solid/liquid ratio, extraction time, agitation, tem­
perature, and others). Fraction (ii) follows a demulsification step to in­
crease the free oil recovery and to produce hydrolyzed compounds (such
as phospholipids, amino acids, and sugars) to be converted into com­
mercial emulsifiers. The solid by-product composition depends on the
raw material but is usually rich in protein or fibers (Souza et al., 2020)
and follows the drying process. The next section addresses how the oil is
stored in the plant tissue and how it directly influences the emulsion
formation on AEP.
3.3. Plant cell structure and its influence on AEP emulsion formation
Triacylglycerol and fatty acids present in oilseeds are developed and
102
Trends in Food Science & Technology 133 (2023) 99–113
stored in embryos and endosperm during seed development. Those
special cell organelles are named oil bodies (OBs) or oleosomes and are
covered with a monolayer of phospholipids embedded with structural
proteins, such as oleosin, caleosins, and steroleosins. Oil bodies are
located inside the plant cell. Plant cell membranes are composed of
phospholipid bilayer and responsible for selective permeability to ions
and molecules between the cell and the environment (Lan et al.,
2020). Proteins bodies (PBs) are also structures present in the vegetable
cell, and these organelles are widely distributed between the cell wall
and the OBs. Fig. 1 illustrates a generic plant cell structure.
In aqueous oil extractions, the proteins act as strong emulsifiers due
to molecular organization, which is formed by long hydrophobic regions
(deeply inserted in the oil body) and an umbrella-like hydrophilic
moiety that connects with the water phase (Sun, Zhang, et al., 2021), as
presented in Fig. 1. In addition, along with oleosin, phospholipids
(monolayer) are the major components of the biological membrane.
They are also formed by a hydrophilic region (which is composed of
glycerol, two fatty acids, and a phosphate group) and a hydrophobic
head group (Zhao et al., 2020). Oleosin and phospholipids (Fig. 1) can
improve the emulsion stability during the AEP, forming a very stable
cream (Cassen et al., 2022). This cellular arrangement to store oil in the
plant tissue should be disrupted to release the oil. The tissue could be
broken by a mechanical process such as milling. Enzymatic treatment is
a valuable tool to boost this disruption. Proteases, phospholipases, cel­
lulases, and amylases can be associated with or even substituted for the
milling step (Díaz-Suárez et al., 2021). Zhang et al. (2020) successfully
applied acidic moisture-conditioning plus low-temperature drying as
pre-treatment on flaxseed kernel before AEP to prevent the emulsion
cream formation and to increase the recovery of the free oil, achieving
83% yield. This effect was attributed to the more efficient comminution
of the flaxseed grains.
The oily fraction resulting from the water extraction can be a very
stable emulsion. The formation of this emulsion could impair the process
scaling up because the recovery efficiency can be lower than the non-
polar solvent procedure and require additional operations to obtain
most of the free oil (Campbell et al., 2011). Emulsion breaking (or
destabilizing the molecules that act as emulsifiers to separate the oil
from water) can be the key to increasing the oil recovery, allowing
further application in oil industries. Also, to be competitive with the
conventional hexane process currently used to produce vegetable oil
around the world, AEP oil extraction yields need to be close to that
obtained with organic solvent extraction (~95%). The AEP yield can
vary according to the demulsification method applied from 23 to 85%,
as indicated in Section 2.
3.4. Emulsion’s systems: A very stable product from AEP
AEP has several advantages, but the emulsification of the extracted
oil during the process can occur. Structurally, emulsions are dispersion
systems constituted by two or more immiscible phases where one liquid
is dispersed as droplets (with different sizes) in another liquid. Emul­
sions can be divided according to the dispersed phase into water-in-oil
(W/O), in which the water droplets are dispersed in the oil phase, and
oil-in-water (O/W), in which oil is dispersed into the water phase (Ma &
Chatterton, 2021). The aqueous oil extraction can yield a cream emul­
sion of oil bodies dispersed in water, characterizing an oil-in-water
emulsion (O/W) (Cassen et al., 2022).
In AEP emulsions, the oil droplets are emulsified by proteins, car­
bohydrates (pectin), and phospholipids (the main constituent of the cell
membrane). A good understanding of microstructural characteristics
and the composition of the major compounds of the selected vegetable
raw material is crucial for understanding AEP limitations. For example,
soybean seeds (a conventional oil source) comprise approximately
18–20% of oil, 40% of proteins (located inside the protein bodies), and
25–30% carbohydrates. The soybean cell wall is constructed of pectin,
hemicelluloses, and cellulose microfibrils (as a primary layer) cross-
G.D. Sorita et al.
Fig. 1. Plant cell structure (Adapted from Nikiforidis et al. (2014)).
linked with proteins (major compound, 40%). As a first stage, breaking
the protein bodies (PBs, with sizes ranging from 2 to 10 μm) is necessary
for the subsequent oil body (OBs, with sizes ranging from 0.2 to 0.5 μm)
breaking. The phospholipid membrane covering the OBs (Fig. 1) hinders
the recovery of free oil (Loman et al., 2018).
It is also important to note that the oil can be found in distinct parts
of the fruits, for example, in the mesocarp and endosperm. A better
understanding of the fruit composition, the microstructure of OBs, and
the compounds that act as emulsifiers in AEP can help choose the
emulsion breaking method and consequently assist in a high oil yield
(Moura et al., 2010). For instance, macaw palm (Acrocomia aculeata)
fruits contain oil in the mesocarp (pulp) and kernel (nut). Macaw
mesocarp and kernel are mainly composed of 38 and 3.5% water, 3 and
28% protein, 29 and 28% oil, 10 and 1% carbohydrates, and 20 and 36%
fibers, respectively (Andrade et al., 2020). In the pulp, OBs (size range
from 0.2 to 2 μm) are scattered and surrounded by fibers (20%). The
kernel also has a large concentration of proteins (28%, stored in indi­
vidualized structures) in the middle of OBs (~20 μm) and inside the cell
wall (Moura et al., 2010; Rosenthal et al., 1996).
Several studies have investigated cream emulsion demulsification
methods such as enzymatic (Hu et al., 2020; Li et al., 2017; Souza et al.,
2020), sonication (Luo et al., 2019), microwave (Hu et al., 2020),
membrane (Moreira et al., 2020), among others. However, the specific
technique to be adopted depends on the vegetable raw material and,
consequently, on the composition of the cream emulsion, which is
strongly affected by the distinction in chemical composition and phys­
ical structure of the oilseeds, and the processing parameters (such as
grinding types and extraction parameters) (Li et al., 2016). A discussion
regarding the main demulsification techniques, advantages, and draw­
backs is presented as follows.
4. Demulsification in AEP: The key step to obtain high oil yields
4.1. Demulsification mechanisms
Several mechanisms have been proposed to describe the demulsifi­
cation process (Kang et al., 2012; Park et al., 2020; Saad et al., 2019).
(i) Creaming and sedimentation: refer to the migration of the phases
due to density differences between water and oil. Since oil is less
dense than water, the oil droplets rise to the surface (creaming),
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Trends in Food Science & Technology 133 (2023) 99–113
and water settles at the bottom of the continuous oil phase
(sedimentation).
(ii) Flocculation: unstable oil droplets or particles in the solution
form aggregates or flocs. This mechanism depends on several
factors, such as water content in emulsions, temperature, oil
viscosity, density, and electrostatic field.
(iii) Ostwald ripening: droplets increase in size due to the diffusion of
smaller oil droplets to large droplets across the aqueous phase.
The process happens as soon as the dispersed phase (oil phase, O/
W emulsion) reaches finite solubility in the continuous phase
(water phase, O/W emulsion). Droplets of different sizes migrate
toward the surface and form the oil top layer.
(iv) Coalescence of the droplets: in this irreversible process, water/oil
droplets fuse or coalesce to form a larger droplet. Factors like
flocculation rate, interfacial tension, interfacial velocity, and
temperature can influence the outcome.
To achieve an effective and robust demulsification process, the
separation of the oil and water phases must occur faster and with a low
content of crude oil in the residual water stream (Saad et al., 2019).
4.2. Common demulsification methods in AEP
Biological, chemical, and thermal treatments have been studied for
cream demulsification from many raw materials (i.e., coconut, soybean,
peanut, moringa and cherry seed, and others) in the AEP process. Some
examples include sonication (Li et al., 2014), microwave (Liu et al.,
2020), heat treatment (Khoei & Chekin, 2016; Zhao et al., 2020),
ethanol adding (Ni et al., 2016), phase inversion (Fang et al., 2016),
freezing-thawing (Zhao et al., 2020), surfactants adding (Geng et al.,
2020), and enzymatic treatment (Hu et al., 2020; Xu et al., 2021). A list
of the most relevant studies regarding demulsification techniques for
conventional and unconventional oil sources is presented in Table 2.
4.2.1. Enzymatic demulsification
Enzymatic treatments were widely applied to break the emulsion
(stabilized by proteins, carbohydrates, and fibers) formed in AEP of
different oil sources, such as palm pulp (Teixeira et al., 2013), rice bran
(Xu et al., 2021), moringa (Yusoff et al., 2016), and bayberry kernels
(Zhang et al., 2012). When AEP uses enzymes, it is called aqueous
enzymatic extraction (AEE). The hydrolytic enzymes are responsible for
G.D. Sorita et al. Trends in Food Science & Technology 133 (2023) 99–113

Table 2
Demulsification methods applied in AEP of conventional and unconventional oil sources.
Demulsification Biomass source Treatment conditions Enzyme action Oil Yield References
technique
a
Enzymatic treatment Moringa Neutrase/Celluclast (3:1 w/w) Neutrase: protease 70% Yusoff et al.
(Moringa oleifera) Celluclast: cellulase (2016)
a
Enzymatic treatment Bayberry (Myrica Cellulose/neutral protease (1:2 w/w) Cellulose: cellalose 31.15% Zhang et al.
rubra) kernels Neutral: protease (2012)
b
Enzymatic treatment Oil palm (Elaeis Pectinase/cellulase/tannase (1:1:1 w/w/ Pectinase: pectinase 90–93% Teixeira et al.
guineensis) pulp w) Cellulase: cellulase (2013)
Tannase: gallotannins and
ellagicittanins
a
Enzymatic treatment Sesame Protex, Alcalase, Viscozyme L, Kemzyme, Protex: protease 57.4% (Alcalase 2.4L) Latif and Anwar
(Sesamum and Natuzyme (2.0%) 45 ◦ C, 120 min Alcalase: protease (2011)
indicum L.) seed 120 rpm Raw material/water ratio: 1:6 Viscozyme L: beta-glucanases,
(w/v) pectinases, hemicellulases and
xylanases
Kemzyme: multi-protease
Natuzyme: phytase, α-amylase,
xylanase, β-mannanase, β–glucanase,
cellulase, protease, lipase and
pectinase
b
Enzymatic treatment Sesame Pectinex and Neutrase (separately, 2% w/ Pectinex: pectinase Neutrase: 89% (1% Pectinex + Tirgarian,
(Sesamum v) and Pectinex (1%) + Neutrase (1%); protease 1% Neutrase) Farmani, &
indicum L.) seed 50 ◦ C for 6 h; Milani (2019)
Raw material/water ratio: 1:1, 2:1, 3:1,
4:1, 5:1 and 6:1 (w/v)
b
Enzymatic treatment Castor (Ricinus Viscozyme L (2% w/w) Viscozyme L: beta-glucanases, 80% Díaz-suárez et al.
communis) seeds Raw material/water ratio 1:5 (w/v) pectinases, hemicellulases and (2021)
xylanases
a
Enzymatic and Yellow mustard Carbohydrase: Viscozyme, Celluclast, and Viscozyme: beta-glucanases, 91% (Protex) Tabtabaei and
chemical treatment (brassica hirta) Pectinex Ultra SP-L (3% w/w), pectinases, hemicellulases and Diosady (2013)
flour xylanases
Proteases: Alcalase, Protex, Protex 51FP, Celluclast: cellulase
and Protex (2.5% w/w)
Chemical treatment: alkaline emulsion Pectinex Ultra SP-L: pectinase
extraction
c
Enzymatic treatment Peanut (Arachis Phospholipase A1 (PLA1), Phospholipase Phospholipase A1, A2 and D: PLA1: 45.6% Niu et al. (2021)
c
hypogea) seeds A2 (PLA2), Phospholipase D (PLD), phospholipase PLD: 30.7%
c
Papain and Alcalase (1.25%) Papain: protease Alcalase: 84.3%
c
Alcalase: endopeptidase Papain: 93.8%
c
PLA1/PLA2: 85.3%
d
Enzymatic and Peanut (Arachis Salts: CaCl2, MgCl2, NaCl Alcalase Alcalase: endopeptidase 92.0% (Alcalase + 5 Zhou et al. (2020)
chemical treatment hypogaea) seeds (0.25–2%, v/v) mM CaCl2)
a
Thermal, chemical Peanut (Arachis Protex 6L, Protex 7L, Protex 50FP, Protex 6L, 7L and 50 FP: protease 92.2% (Protex 50FP) Li et al. (2017)
and enzymatic hypogea) seeds Alcalase 2.4L, Papain, phospholipase, and
treatments Amylase at 1.5% (w/w).
Raw material/water: 1:5 (w/v); Alcalase: endopeptidase Papain:
protease
NaOH (2 mol L− 1) Phospholipase: phospholipase
50–60 ◦ C Amylase: amylase
b
Enzymatic and Camellia Neutral protease/Cellulose (6:5 w/w), 40 Neutral: protease Cellulose: cellulase Microwave: 83.05% Yang et al. (2019)
b
thermal treatment (Camellia oleifera min; Freezing/thawing:
Abel.) seeds − 20 ◦ C/50 ◦ C (2 cycles) 89.37%
Microwave: water/raw material ratio of
1:4 at 50 ◦ C, pH of 6.5, 0.9% (w/w)
b
Chemical treatment Camellia Surfactant: Tea saponin 1:5 (w/w) – 89.62–93.58% Zhang et al.
(Camellia oleifera (2019)
Abel.) seeds
b
Chemical and Almond (Prunus Neutral Protease Neutral: protease 65% (by both Dias et al. (2020)
Enzymatic dulcis L.) flour Solids/liquid ratio of 1:10 (w/v), 120 rpm treatment)
treatments at 50 ◦ C.
Chemical demulsification: at pH 5.0
(almond protein isoelectric point)
b
Chemical treatment: Walnut (Juglans Sodium chloride solution (0.6–1.4 mol – 91.2% (Chloride Geng et al. (2020)
Surfactant and salt regia L.) kernels L− 1); solution)
adding Span 20, Span 80,Tween 20, and Tween
80
a
[mass of extracted oil (g)/mass of dry raw material (g)] * 100.
b
[mass of extracted oil (g)/mass of oil in dry raw material by solvent extraction (g)] * 100.
c
[free oil from emulsion (g)/mass of oil in the emulsion (g)] * 100.
d
Mass of free oil (g)/[mass of cream (g) * oil content by solvent extraction (%)].

104
G.D. Sorita et al.
breaking the natural surfactants (proteins, phospholipids, and carbo­
hydrates present in the raw material) that stabilize the cream emulsion
into small molecules (peptides, mono or disaccharide, and others), dis­
placing and coalescing the emulsion droplets (Li et al., 2017).
Enzyme-assisted processes usually are considered more expensive due to
the cost of enzymes. However, it is worth noting that the AEP assisted
with phospholipases, could eliminate the degumming steps in oil
refining since this enzyme converts nonhydratable phospholipids into
lysophospholipids, which are insoluble in oil and removed in the
aqueous fraction after centrifugation steps (Gharby, 2022).
AEE can reach high yields and produce high-quality oil (considering
sensorial and technological parameters) suitable for human consump­
tion. The use of enzymes in demulsification steps positively influenced
the sensory and technological aspects of different oils, which can
favorably affect the final product in terms of taste, smell, and color
(Yusoff et al., 2015). The camellia seed oil extracted with AEP and AEE
was less colored and brighter when compared to oils extracted through
mechanical pressing (Yang, Zhao, Fan, Deng, & Xiong, 2012). Sensory
analyses (taste, odor, and color) of sesame seed oil extracted by AEE and
SE showed high acceptability of AEE oil compared to SE. Besides,
Najafian et al. (2009) reported that olive oil turbidity decreased with
pectinase use, which may be due to the enzymatic effect in reducing the
number of colloidal particles in olive oil. Other benefits can be achieved
when enzymes are applied to the demulsification step in AEP, including
low chemical pollution, low energy consumption, and good retention of
protein, polysaccharides, fibers, and phytochemicals, which can further
be used in a biorefinery concept in food or pharmaceutical industries
(Yusoff et al., 2015).
Commercial enzymes such as Alcalase (Latif & Anwar, 2011; Niu
et al., 2021; Xu et al., 2021), Protex, Viscozyme, Kemzyme, and
Naturazyme (Latif & Anwar, 2011), Celluclast (Tabtabaei & Diosady,
2013), Phospholipase A1, A2, and D types, papain (Niu et al., 2021),
amylase (Li et al., 2017), and others have been widely applied in blends
or separately for distinct vegetable sources, as shown in Table 2. The
applicability of Viscozyme L (an enzyme cocktail containing xylanase,
arabanase, β-glucanase, hemicellulose, and cellulase activities) by Día­
z-Suárez et al. (2021) shows a successful cream demulsification formed
in the AEP process using castor seed, reaching high oil yield (80%) with
the same fatty acid composition and with better oxidative stability than
organic solvent extraction.
AEP emulsion is stabilized by more than one type of surfactant
(usually proteins, phospholipids, fibers, and carbohydrates). Therefore,
according to the plant cell composition, one or more enzymes must be
applied to achieve complete demulsification and, consequently, high oil
yield. For example, papain (a proteolytic enzyme) applied in peanut
cream can lead to an oil recovery of 93.8% (Niu et al., 2021). In this case,
the high protein content with remarkable emulsifying properties in the
seed is responsible for stabilizing the emulsions formed in the process.
On the other hand, for Moringa oleifera seeds (also with high protein
content but with low emulsifying ability), the high oil recovery (70%)
was achieved using a blend of cellulase and protease (3:1 w/w) since the
cellulose is the most compound responsible for emulsifying the oil
(Yusoff et al., 2015).
4.2.2. Thermal demulsification
This technique involves changing the emulsion’s temperature to
separate the oil and water phases. In this method, a high temperature
(50–60 ◦ C) is applied to reduce the rigidity of the emulsion interface,
decreasing the emulsion stability, and increasing the collision between
the droplets, making it easier for droplets to coalesce (Abed et al., 2019).
Freezing-thawing and microwave integrated with other methods (such
as enzymatic and salt addition) are the thermal techniques most applied
in AEP, and camellia seeds (Yang et al., 2019), peanut seeds (Liu et al.,
2020) and rapeseed (Tian et al., 2019) are some examples. This method
consists in freezing and subsequently thawing the cream emulsion. The
fundamental freezing-thawing mechanism is explained by Yuan et al.
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Trends in Food Science & Technology 133 (2023) 99–113
(2021). Briefly, when the oil-in-water emulsion (O/W) is gradually
frozen, the oil crystals move to the oil droplets’ interfaces, inducing their
partial coalescence and forming oil aggregates that decrease the stability
of the emulsion. Simultaneously, the volume expansion caused by the
phase transition of water moves the oil droplets to get closer, thus
making them more prone to coalescence while they are thawed. The
freezing-thawing treatment effectiveness has been reported in a study
conducted by Yang et al. (2019) that evaluated the demulsification of
the cream emulsion obtained by AEP from camellia (Camellia oleifera
Abel.) seeds using frozen (− 20 ◦ C) and thawing (50 ◦ C) treatments,
reaching 89.37% of oil extraction yield.
Microwave applies non-uniform heating near the droplet surface,
forming an electromagnetic field with a high-frequency variation. The
droplet, at high-speed rotation, destroys the interface film (due to their
collision), causing emulsion breaking and droplet coalescence, allowing
the oil separation. Usually, microwave demulsification is assisted by
other techniques, such as enzyme or salt addition (Kovaleva et al., 2018;
Liu et al., 2020). The integration of more than one demulsification
method is described in Section 4.2.4.
The thermal demulsification method has also been used by an
increasing number of researchers in wastewater treatment and petro­
leum industries, owing to its simplicity and efficiency. The main draw­
back of thermal demulsification in food applications is the high
temperatures (50–60 ◦ C) needed, which can degrade unsaturated fatty
acids and bioactive compounds. However, the temperature increase can
influence the oil’s oxidative stability (reducing its quality) and cause
protein denaturation, hindering further use of the protein fraction.
Optimizing the right temperature and time is essential for minimizing
losses (Saad et al., 2019).
4.2.3. Chemical demulsification
Chemical demulsification has been extensively applied in the AEP,
petroleum industries, and wastewater treatment with good effectiveness
and cost-efficiency for breaking emulsions (Dias et al., 2020; Wang et al.,
2021). Chemical demulsification uses chemical additives to accelerate
the emulsion-breaking process (Dias et al., 2020). The chemical addition
(salts and surfactants) is designed to neutralize the effect of the mole­
cules that act as emulsifiers stabilizing the emulsion (proteins, carbo­
hydrates, fibers in AEP). The added compound displaces the emulsifier
from the interfacial film surrounding the emulsion droplets to enhance
destabilization, resulting in droplet coalescence (Yonguep et al., 2022).
For an efficient chemical separation, a chemical additive (sodium
chloride solution, span 20, span 80, tween 20, tween 80, tea saponin,
and others) in an adequate amount must have the capacity to demulsify
emulsions within an optimized residence time (Wang et al., 2021). The
mechanism behind thermal and chemical demulsification integration is
presented in the next section (section 4.2.4). In addition, the oil fatty
acid composition, viscosity, emulsion size, and the presence of solids can
influence the efficiency of the process (Abed et al., 2019). This demul­
sification method is usually applied along with a thermal demulsifica­
tion step and can achieve high (>85%) or moderate (60–85%) oil
recoveries. Dias et al. (2020) reached an oil recovery of 69.3% from AEP
of ground almonds by applying chemical demulsification on the cream
emulsion obtained after the centrifugation step by adding 2 mol L− 1
NaOH (pH at 5) under 57.5 ◦ C for 37.5 min. High oil recovery
(89.62–93.58%) from Camellia seeds was obtained by Zhang et al.
(2019) by recirculating tea saponin (an abundant natural nonionic
surfactant presented in Camellia seeds) accumulated in the aqueous
phase in the cream emulsion fraction, reducing the products costs and
wastewater output. Geng et al. (2020) obtained a reasonable oil recov­
ery (91.2%) from walnut seed using sodium chloride solution (1.2 mol
L− 1) and Span 20 (1.7 g 100 g− 1) in the extraction steps (before
centrifugation) under 85 ◦ C for 60 min.
4.2.4. Integration of traditional demulsification methods
Integrating two or more traditional demulsification methods is
G.D. Sorita et al.
essential for improving the emulsion breaking. The applicability of the
integrated demulsification processes can be seen in the study by Liu et al.
(2020). These authors tested microwave demulsification (thermal
treatment) with salt addition (chemical treatment) for peanut oil
extraction. The microwave heating with CaCl2 addition presented a high
oil recovery (92.30%) compared to conventional microwave heating
(46.86%).
Using inorganic salts in small quantities can increase the water
conductivity and thereby increase the microwave radiation in the
demulsification process. This effect occurs mainly at low microwave
frequency, where the contribution of the conduction mechanism pre­
dominates in dielectric heating. The inorganic salts can neutralize the
surfactants, which stabilize the emulsion and displace them from the
interfacial film surrounding the emulsion droplets to promote destabi­
lization and, consequently, the oil separation (Wang et al., 2021).
Salt addition can also be integrated with enzyme demulsification
(biological treatment). In AEE, the proteolytic enzyme can hydrolyze
proteins into small peptides, which release the oil fraction from the oil
bodies. Although peptides act as emulsifiers in the cream fraction,
adding salt (NaCl, MgCl2, CaCl2) at a low concentration induces to reach
the isoelectric point; the peptides start to aggregate, releasing the oil and
yielding the oil-free fraction (Zhou et al., 2020). Similar oil yield in AEE
can be achieved by reducing the enzyme quantity 62.5 times and adding
CaCl2 (5 mM) in peanut oil extraction (Zhou et al., 2020).
5. Upgrading demulsification methods in AEP: The possibilities
of physical demulsification methods
Physical demulsification methods have been studied for wastewater
treatment and in the petroleum industry (Ajogbeje et al., 2021; Naga­
sawa et al., 2020; Yang et al., 2020) and could be applied in the food
industry. The methods are recognized for their high efficiency, fast
separation time, environmental friendliness, and for being performed
with no addition of enzymes and chemicals. Physical methods can be
divided into two major groups (Fajun et al., 2020): (i) governed by an
external force – centrifugation, gravity sedimentation, membrane (Del
Colle et al., 2007), vibration, and coalescer separator (Ajogbeje et al.,
2021); and (ii) governed by energy application (waveform) – ultrasonic
(Luo et al., 2019) and electric (Lu et al., 2021).
The olive and avocado oil extraction industries have used centrifugal
decanters to improve the oil separation in aqueous extractions. How­
ever, the olive or avocado paste must be diluted with warm water to
reduce the viscosity of the solid phase and improve oil separation. The
amount of contaminated wastewater produced by this process is corre­
spondingly increased and could be as high as 50% of the mass of the raw
material processed, posing an ecological problem. A large amount of
water added to the process leads to a considerable reduction in the
natural antioxidant in the resulting oil (Permal et al., 2020; Tamborrino
et al., 2015). In this sense, the proposed new physical demulsification
methods (such as filter-coalescers and membranes) may be an attractive
alternative to traditional equipment such as the horizontal decanter
centrifuge.
The mechanism involved in the innovative physical methods pro­
posed is simple and adjusted to the required needs of each process. The
filter-coalescer and membrane can be produced by changing the
porosity, pore diameter, and charge according to emulsion size and the
composition of the raw material used in the process, increasing the
equipment’s functionality. Considering a hydrophilic layer (filter-coa­
lescer and membrane) and an oil-in-water (O/W) emulsion, water
molecules can adhere to the filter or membrane pore surfaces, increasing
permeability. The entrapped water (and soluble hydrophilic compounds
that act as emulsifiers, such as sugars, amino acids, and others) acts as a
repulsive phase for the oil droplets contacting the membrane. The
increased contact of small oil droplets caused by the water flow through
the membrane pores leads to the coalescence of the oil phase. Filter-
coalescers and membrane pores allow water permeation;
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Trends in Food Science & Technology 133 (2023) 99–113
consequently, they resist the oil droplet’s passing. As a result, oil and
water separate from the emulsion. The opposite effect occurs if the
equipment (filter-coalescer/membrane) has a hydrophobic layer (Yadav
et al., 2022).
The considerable interest in physical demulsification can be justified
by its flexibility since the composition of unconventional oil matrices
worldwide varies significantly. Moreover, the filter-coalescer and
membrane surface characteristics can be adjusted for treating oil from
diverse sources. Positive impacts in extraction oil processing and pres­
ervation can be achieved, such as higher oil yields and relatively shorter
processing times (since the solvent does not dissolve the oil, and the
process does not require solvent removal post-steps). Additionally, no
thermal or chemical treatment is required, helping to keep the initial oil
quality (quality similar to the in-nature pulp). However, it is worth
noting that the porous beds need to be food-grade to ensure food safety,
which may increase production costs.
To the best of our knowledge, literature data does not report
demulsification methods by membranes and coalescers in AEP for edible
oil extraction. Thus, it is important to briefly discuss this method and the
technologies used in other areas to advance studies in the food industry
field. Table 3 lists studies on physical demulsification applied in
wastewater treatment and petroleum industries.
5.1. Filter-coalescers
Filter-coalescers use physical means to induce oil coalescence and
produce a continuous separation of oil and water in distinct phases. Five
conventional mechanical coalescence separator categories can be found
in the literature: gravitational, plate, packing type coalescing separators,
coalescing filter separators, and fibrous separators (Almeida, Esquerre,
Soletti, & Silva, 2019; Lu et al., 2019). The filters are arranged inside
compact equipment (mechanical coalescer) and have a high separation
efficiency. This technique can efficiently separate emulsions with
droplet sizes smaller than 10 μm, achieving high yields at a low capital
expenditure in continuous operation and allowing a large-scale appli­
cation (Kumar et al., 2021). In addition, the equipment is easy to install,
automatize, self-clean, and operate with simple maintenance (Ajogbeje
et al., 2021).
Filter coalescers have been successfully applied in the petroleum
industry and wastewater treatment in the food industries. They are
mostly applied for emulsions with droplet sizes smaller than 10 μm. For
instance, Ajogbeje et al. (2021) studied the application of a fibrous
filter-coalescer to promote the coalescence and separation of
water-in-bitumen (water-in-oil) emulsion (>10 μm), achieving a
reduction of water content in the emulsions from 2 vol% to 0.1 vol%. Lu
et al. (2019) proposed and applied (in an offshore platform) a system
composed of a fibrous filter-coalescer for the demulsification of petro­
leum wastewater (with emulsion size >10 μm), obtaining efficiency
higher than 98%. The authors also presented the microscopic mecha­
nism and a theoretical model for calculating the separation performance
that may improve industrial applications. A proposed mechanism of
horizontal bed coalescers for AEP can be seen in Fig. 2 (A), in which the
emulsions formed during AEP (oil, water, protein, phospholipids, car­
bohydrates, and fibers) are fed in the top left side and are induced to pass
through one or more porous beds that retain and coalesce the small
droplets.
The large droplets are then pushed outside the bed by dynamic forces
and gravity. The oil phase remains in the top (upper part) of the mixture,
and the water phase (in the AEP case, with the surfactants – proteins,
phospholipids, carbohydrates, and fibers) is further separated (Almeida
et al., 2019; Lu et al., 2019). It is important to note that the water phase
(bottom of the coalescer) contains valuable compounds such as soluble
sugar, amino acids, and pectin that can be further separated and used in
food applications, fitting a biorefinery concept.
Applications of filter coalescers in AEP were not reported in the
literature data so far. The size of the emulsion droplets in AEP changes
G.D. Sorita et al. Trends in Food Science & Technology 133 (2023) 99–113

Table 3
Most relevant works related to physical demulsification applied in wastewater treatment and petroleum industries.
Physical type Application/ Filter-coalescer/membrane type Emulsion Results Reference
Emulsion

Filter-coalescer Water/bitumen Fibrous Filter-coalescer Water/bitumen emulsion Reduction of water content Ajogbeje et al.
emulsion (W/O) in emulsion: 2 vol % to 0.1 (2021)
vol %.
a
Wastewater (O/ Fibrous Filter-coalescer Diesel oil droplets, methyl silicone oil Efficiency: >98% Lu et al. (2019)
W) droplets, dibutyl phthalate droplets
a
Filter-coalescer Wastewater (O/ Coalescer bed: cationic exchange resins Effluent of the petroleum industry Efficiency: >93% Motta et al.
integrated W) Membrane: a polyetherimide hollow fiber (2014)
with submerged module (hydrophilic
membrane membrane)
a
Membrane Wastewater (O/ Aramid nanofibers membrane modified Lubricating oil or diesel or N- Efficiency: 99.73% Guan et al.
separation W) with β-cyclodextrin (hydrophilic hexadecane or soybean oil + Tween Permeate Flux: 126.59 L (2021)
membrane) 60 and Sudan III + deionized water m− 2 h− 1
a
Biodiesel Aluminum titanium oxide powder tubular Biodiesel Efficiency: >99.73% Moreira et al.
purification (O/ ceramic membranes (pore size/Molecular (2020)
W) weight cut-off: 0.05 μm/20 kDa)
(hydrophilic membrane)
a
Wastewater (O/ Polydopamine microspheres integrated Sodium lauryl sulfonate + deionized Efficiency: >99.9% He et al. (2019)
2
W) with polyacrylonitrile nanofibers water + toluene Permeability: 11666 L m−
membrane (pore size: 300 nm) h− 1 bar− 1
(hydrophilic membrane)
a
Wastewater (O/ Poly (vinylidene difluoride) modified with Canola oil + tween + water Efficiency: ~98% Zin et al. (2019)
W) dopamine and polyethyleneimine
membranes
(pore size: 0.1 μm) (hydrophilic
membrane)
Wastewater (O/ Gutta-percha (natural polymer)/silylated Petroleum ether, dichloromethane or Highly effective oil-water Yang et al. (2020)
W) nanofibers membranes (hydrophilic toluene, or cyclohexane + deionized emulsions separation with
membrane) water permeate fluxes of:
Petroleum ether: 3624 L
m − 2 h − 1 W− 1
Dicholomethane: 3308 m− 2
h − 1 W− 1
Toluene: 3186 m− 2 h− 1 W− 1
Cyclohexane: 2866 m− 2 h− 1
W− 1
a
Oil spill (O/W) Electrospun fibers of polycaprolactone Hexadecane + span 80 and Tween 80 Efficiency: >99.0% Panatdasirisuk
Membranes with Anisotropic Pores + deionized water Permeate flux: 70 L m− 2 h− 1 et al. (2017)
(porosity: 88% and pore size: 359–272 bar− 1
nm) (hydrophilic membrane)
a
Wastewater O/ Poly (vinylidene fluoride) modified with Sodium lauryl sulfonate + soybean oil Efficiency: >85% Xiong et al.
W polydopamine/polyethyleneimine and + sodium lauryl sulfonate or stearyl (2020)
Fe2+(hydrophilic membrane) trimethyl ammonium or tween 40 +
deionized water
a
Wastewater (O/ Attapulgite − graphene oxide composites Heavy crude oil + ultrapure water Efficiency: >95% Liu et al. (2021)
W) (hydrophilic membrane)
a
Efficiency: relation between oil content in the aqueous phase before emulsion separation and the oil content in filtrate after emulsion separation.

according to the raw material and the process parameters, and it usually
is in the range of 2–10 μm (Zhang et al., 2013). Thus, a filter-coalescer
efficiently separates emulsions from AEP with a droplet size smaller
than 10 μm.
5.2. Membrane
Membrane-based processes such as microfiltration and ultrafiltration
are an alternative for oil/water separation since selective barriers are
used to separate feed species into two phases, driven by a hydraulic
pressure application (Xiong et al., 2020; Yang, Wen, et al., 2021). Both
O/W and W/O emulsions can be separated, and the use of specific
membranes for each case (Fig. 2 (B)) is recommended: (i) membranes
with (super)hydrophobic surfaces (surfaces with oil affinity) and (ii)
membranes with (super)hydrophilic surfaces (surfaces with water
affinity).
Advantages of membrane technology include environmentally
friendly (chemicals are used only in cleaning procedures); operation at
mild temperature (protecting oil characteristics); energy-efficient (no
phase change); continuous or batch process; low maintenance, and easy
operation (Panatdasirisuk et al., 2017). The main limitation of mem­
brane separation is the fouling (accumulation of particles or solutes in
the membrane pores and on the surface), which affects the process
performance in terms of permeate flux and quality (Xiong et al., 2020;
Yang, Wen, et al., 2021).
The literature has constantly addressed membrane processes’
demulsification of O/W and W/O emulsions. Most studies focus on O/W
emulsion for biodiesel, wastewater treatment, and the petroleum in­
dustry (Table 3). For instance, Moreira et al. (2020) applied a tubular
ceramic membrane to improve biodiesel quality (improving glycerol
separation). A study by Nagasawa et al. (2020) evaluated the filtration
performance of porous ceramic membranes to treat O/W emulsions and
concluded that surface charge and pore size were the two most impor­
tant parameters influencing fouling during O/W demulsification.
The droplet size of AEP emulsions (2–10 μm) is similar to the droplet
sizes of the emulsions from the studies in other areas (Zhang et al.,
2013), thus membrane technologies can be adapted for breaking the
emulsions formed in AEP. A pre-treatment can also be an alternative for
emulsions with larger droplet sizes. For example, since filter coalescers
can efficiently separate emulsions with droplet sizes up to 10 μm (Kumar
et al., 2021), they could be used as the first step for treating a coarse
emulsion. Then, membrane separation could be used for treating the
aqueous stream containing smaller oil droplets, enhancing the process
efficiency.

107
G.D. Sorita et al. Trends in Food Science & Technology 133 (2023) 99–113

The vegetable oils for human consumption are standardized by

composition and quality. According to Codex Alimentarius (1999),
several physical and chemical parameters are used to monitor the
identity and quality of a specific crude or refined vegetable oil. In terms
of composition, the fatty acid determines the identity, i.e., the species
from which a given oil is derived. For quality assessment, several
physicochemical parameters are evaluated, such as moisture and vola­
tile matter at 105 ◦ C, iodine index, insoluble impurities, soap content,
relative density, refractive index, saponification value, peroxide value,
and free fatty acids. Other minor compounds are also assessed, such as
sterols and tocopherols.
Interestingly, the oil obtained in AEP from different raw materials
presents higher quality than those obtained by pressing and solvent
extractions (Niu et al., 2021; Santos et al., 2022; Zhou et al., 2020).
Consequently, some studies suggest that the refining process may be
unnecessary or less intense (Hadi et al., 2021; Yang et al., 2019). The
high oil quality obtained in AEP was observed by Tirgarian et al. (2019),
who compared the oil quality obtained from sesame seed by AEE and by
solvent-extraction (Soxhlet with hexane) without the refining process.
The AEE oil presented better physicochemical properties (such as iodine
and saponification value, free fatty acid, moisture, unsaponifiable con­
tent, color, phenol content, peroxide, and anisidine value) than the oil
obtained with solvent extraction. The same result was observed by
Díaz-Suárez et al. (2021), which used enzymes for the cream demulsi­
fication of AEP from castor seeds. They justified the higher oil quality
(compared with solvent extraction) by the simultaneous extraction of
phenolic compounds and tocopherols, which can act as antioxidant
compounds and improve the oil’s oxidative stability.
AEP and solvent extraction (n-hexane) for rice bran oil were
Fig. 2. Suggestion of a physical demulsification mechanism of the cream from
AEP and its products in (A) filter-coalescer and (B) membrane separation.
compared by Xu et al. (2021). The acid value (7.97 and 8.29 mg KOH
g− 1, for AEP and solvent extraction, respectively) presented no signifi­
cant difference between the extraction methods. AEP oil presented a
Another relevant parameter to consider is the emulsion viscosity,
significantly higher saponification value (184.87 and 178.66 mg KOH
which influences the membrane flux (high for oils with low viscosity)
g− 1 for AEP and solvent extraction, respectively) and iodine value
(Tao et al., 2014). For example, using a hydrophilic membrane, an O/W
(106.31 and 102.22 mg I2 g− 1 for AEP and solvent extraction, respec­
emulsion formed with soybean presented high viscosity (8.5 mPa s) and
tively) than solvent extraction. Conversely, AEP presented a signifi­
a low permeate flux (8338 L m− 2 h− 1). This effect is explained by the
cantly lower peroxide value (8.15 mmol kg− 1) than solvent extractions
accumulation of the oil (as a barrier layer) hindering water permeation
(8.80 mmol kg− 1). AEP has also been shown to be better than solvent
(Tao et al., 2014). Considering that the product formed in AEP may
extraction for macaw oil in terms of acidity, leading to 10 times lower
present high viscosity (differing from the vegetal raw material used),
acidity (0.4 oleic acid %) than solvent extraction (4.2 oleic acid %)
some studies have proposed developing special membranes to separate
(Favaro et al., 2022).
high-viscosity emulsions. For instance, Sun, Zhang, et al. (2021) pre­
Zhang et al. (2019) and Geng et al. (2020) also studied the quality of
pared attapulgite-coated polyacrylonitrile nanofiber membranes that
the oil obtained with AEP using chemical demulsification to enhance oil
showed anti-fouling properties and efficient separation (higher than
yields for Camellia seeds and walnut. Both studies showed that the oil
99.4%) of high-viscosity O/W emulsion (kerosene or crude oil or
quality from AEP was better than solvent extraction without refining
n-hexane or petroleum ether or n-heptane, deionized water, and Tween
post-treatment. In addition, Zhang et al. (2019) submitted the oil ob­
80).
tained in AEP to a refining process and observed that the refined oil did
Therefore, a complete study of the emulsion systems obtained in AEP
not present significant changes compared to non-refined oil. Also, the
can provide essential information for selecting the appropriate mem­
unsaturated fatty acid contents were higher in non-refined oil.
brane for each oil source since its composition (protein, fibers, carbo­
A recent study by Hou et al. (2020) demonstrated that membrane
hydrates) differ according to the raw material applied, facilitating
degumming of crude rapeseed oil efficiently removed the phospholipids
process optimization and, consequently, an efficient separation with
and water and was beneficial for decreasing free fatty acids and peroxide
higher oil yields (>95%). Moreover, information regarding the mem­
value. Similar results were found by Azmi et al. (2015), that applied a
brane pore size has been neglected in several papers related to the
polyvinylidene fluoride membrane modified by polyvinyl alcohol to
physical demulsification of oils, indicating the need for further studies.
enhance the interaction between the membrane and the free fatty acid
molecules. The membrane exhibited the highest free fatty acid rejection
6. Refining process and quality parameters
(5.93%) and, at the same time, reduced its color intensity with no
chemical additives. This promising result shows that physical demulsi­
A robust refining process is required to guarantee the safety of the oil
fication (such as filter-coalescers and membrane) can improve the oil
obtained by conventional methods. The refining process comprises: (i)
quality from AEP and, at the same time, remove phospholipids with the
degumming: which removes gums and phosphatides insoluble in the oil;
water, without the need of a refining processes.
(ii) neutralization: which removes free fatty acids, color bodies, and
In summary, AEP with no chemical or thermal treatment may pro­
metallic pro-oxidants; (iii) bleaching: which removes pigments and
vide a higher oil quality in terms of phenolic compounds and unsatu­
traces of residual soaps; (iv) deodorization: removes free fatty acids and
rated fatty acids without needing refining since conventional thermal
oxidative products, such as aldehydes and ketone and undesirable flavor
and chemical oil exposure can degrade the phenolic compounds and
components (Cervantes-Paz & Yahia, 2021).
unsaturated fatty acids, increasing the rate of oil oxidation.

108
G.D. Sorita et al.
7. Upgrading the aqueous oil recovery process (AEP) and the
possibility of by-products uses in a biorefinery approach
A generic industrial process for oil production from conventional or
unconventional oil sources was suggested, considering the aspects
related to enhancing the oil recovery by aqueous oil extraction pro­
cessing, the demulsification techniques, and the by-products generated
in the process. It is important to emphasize that the process can be
adapted according to the oil source. The proposed generic design for
industrial oil production by aqueous oil extraction is presented in Fig. 3,
which shows the possibilities for enhancing oil recovery by integrating
physical demulsification techniques (coalescer and membranes).
Furthermore, this process also suggests the possibility of complete uti­
lization of the by-products generated in the process, reaching a “zero
waste production” and a biorefinery approach.
For instance, to enhance the oil separation and overcome the oper­
ational limitation of coalescer beds and microfiltration membranes
(when applied separately), Motta et al. (2014) integrated both processes
for higher oil removal from wastewater. They proposed two stages: (i)
the emulsions (with oil droplets ranging from 3 to 8 μm) were submitted
to a coalescer bed (formed by a cationic exchanging resins), and then the
water phase (still with a significant amount of oil droplets) was directed
to the second stage, (ii) using microfiltration. The latter was carried out
with a polyetherimide hollow fiber with a permeation area of 0.5 m2.
The coalescer bed (applied separately) efficiency did not achieve the
best efficiency, ranging from 35 to 52%. However, the integrated pro­
cess shows to be promising, achieving high efficiency of oil separation,
ranging from 93 to 100%. These sequential demulsification processes
effectively demulsified wastewater (with similar behavior to the cream
obtained in AEP), suggesting they could be applied to the demulsifica­
tion of other emulsion types, such as those obtained in AEP. In­
vestigations about techno-economic aspects of integrating more than
Fig. 3. Generic biorefinery design for industrial oil production by aqueous oil extraction based on physical demulsification methods.
109
Trends in Food Science & Technology 133 (2023) 99–113
one physical demulsification process (filter-coalescers and membrane
separation) in continuous operation should be performed to assess the
capital and operational expenditures to support the industrial process
feasibility.
Multiple products can be obtained from the solid phase, as shown in
Fig. 3. This phase is composed mainly of proteins, fibers, and carbohy­
drates with biological properties that can be used as ingredients in
numerous formulations in the food industry, such as protein based-
product, emulsifiers, and prebiotics. The by-products can be used
(separated or in the crude form) for food formulations, for example,
enriching cookies (Li, Sun, et al., 2020), production of astaxanthin for
antioxidant uses (Harith et al., 2019), developing healthier fiber-rich
meat products (Sánchez-Zapata et al., 2010) and others. The water
phase (at the final of membrane separation) can be a source of proteins,
carbohydrates, and hydrolyzed fibers (by the milling pre-treatment) that
can be further used as a functional and nutritional ingredient in acidic
beverages, cereal products, food emulsions (as emulsifier) and micro­
biological agents (Tirgarian et al., 2019). Additionally, depending on the
raw material composition and particle size, the water phase can be used
without pre-treatment to produce bioproducts by fermentation pro­
cesses (Favaro et al., 2022), minimizing the effluent treatment drawback
as Rosenthal et al. (1996) reported, as mentioned in section 5. This
important tool can add value to those industries and consequently fit
into a global biorefinery market (Ajogbeje et al., 2021; Almeida et al.,
2019; Kumar et al., 2021; Panatdasirisuk et al., 2017; Xiong et al., 2020).
Besides, the non-edible parts from the vegetable oil sources (husk
and endocarp) can contribute to this chain by producing other high-
added value products, such as bio-energy, bio-ethanol, adsorbent ma­
terial, bio-compounds (phenolic compounds), antibiotic, bio-fertilizer,
bio-polymer, enzymes, and other products (Barbosa et al., 2022; Sar­
kar et al., 2021; Sorita et al., 2020; Ye et al., 2020).
This system could be a suitable approach for conventional oil
G.D. Sorita et al.
extraction based on a green process. The proposed system applies
renewable plant resources (unconventional sources), alternative recy­
cling solvents (water), and the production of co-products instead of
wastes. Additionally, it reduces unit operations (eliminating the refining
oil steps), eliminates the use of chemical additives and temperature
changes, and follows the principles of the circular economy (Chemat
et al., 2019, 2020; Sorita et al., 2022).
In the near future, an industrial process that adopts the biorefinery
concept can lead to the achievement of a sustainable green concept with
lower environmental impact and generally with high-quality products
(Sorita et al., 2020).
8. Conclusions and outlook
With the increase in global warming concerns, biofuels emerge as a
solution for decreasing the exploitation of carbon sources. Conse­
quently, it leads to a direct competition of land required for the con­
ventional crops used for oil production in food industries. In this sense,
some emergent unconventional oil sources and greener extraction pro­
cesses have gained attention. The conventional methods applied for oil
recovery usually have high energy demand and require a large volume
of toxic solvents. AEP is a recent technology used to simultaneously
extract oil and other compounds, such as protein and phospholipids,
from different biomasses. Its industrial applicability requires low in­
vestment and operational costs. The main drawback is that a very stable
cream emulsion is formed, which may require demulsification methods.
So far, only standard demulsification methods have been investigated.
Physical methods such as filter-coalescers and membranes are still
poorly investigated in the demulsification of AEP fractions and present
prominent potential. New studies should focus on demulsification in
AEP to produce high-quality edible oil in food-grade environments and
food safety. The industrial interest in replacing non-environmentally
friendly processes gives industrial reliability to expand new demulsifi­
cation technologies for filter coalescers and membranes. This review
also provides a perspective of an industrial process, fitted in a bio­
refinery approach, with multi-product production and no waste gener­
ation, as an opportunity to aggregate value in oil industries, following
the principles of the circular economy.
Declaration of competing interest
None.
Data availability
No data was used for the research described in the article.
Acknowledgments
The authors acknowledge the National Council for Scientific and
Technological Development (CNPq, # 400092/2020-4, 307576/2018-3,
420275/2018-5, 477497/2013-6, 552185/2011-6), Coordination for
the Improvement of Higher Education (CAPES, PROEX), and Ministry of
Agriculture, Livestock, and Food Supply (MAPA, 21000.074917/2019-
39) for financial support. We would like to thank Katherine Phillips for
proofreading the manuscript.
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