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Subcritical Extraction of Oil from Black and White Chia Seeds with n -propane
and comparison with conventional techniques

Article  in  Journal of Supercritical Fluids The · June 2018

DOI: 10.1016/j.supflu.2018.06.017

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 The Journal of Supercritical Fluids 140 (2018) 182–187

Contents lists available at ScienceDirect

The Journal of Supercritical Fluids

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

Subcritical extraction of oil from black and white chia seeds with n-propane T
and comparison with conventional techniques
⁎
Maša Knez Hrnčiča, , Darija Cöra, Željko Kneza,b
a
University of Maribor, Faculty of Chemistry and Chemical Engineering, Smetanova 17, SI-2000 Maribor, Slovenia
b
University of Maribor, Faculty of Medicine, Taborska ulica 8, SI-2000 Maribor, Slovenia

G R A P H I C A L A B S T R A C T

A R T I C LE I N FO A B S T R A C T

Keywords: Subcritical fluid extraction from Chia seeds (Salvia hispanica L.) using n-propane as a solvent and classical ex-
Extraction tractions as Soxhlet and ultrasonic extraction in n-hexane were performed to obtain oil rich extract. Influence of
Supercritical fluids elevated operating pressure (up to 300 bar) and temperature (40 °C and 60 °C) on the extraction yield and extract
Chia composition is presented. Higher solvent density contributed to higher extraction yield, which increased from
Linolenic acid omega-3
14.38% to 20.8%. Extraction kinetic curves were modelled using Brunner’s equation and the model has been
Linoleic acid omega-6
proved to fit well to the results. Compositions of extracts obtained by different methods were analysed and
compared by gas chromatography (GC). Presence of palmitic, stearic, oleic, linoleic and linolenic free fatty acid
has been confirmed. The highest proportion of linolenic (almost 60%) and linoleic acid is attained in oils ob-
tained by subcritical propane extraction.

1. Introduction
In recent years, there has been a growing interest and promising
development of unusual plants as alternative sources of vegetable
dietary components. Chia (Salvia hispanica L.) has been among the
principal crops grown by ancient Mesoamerican cultures, but dis-
appeared for centuries until the middle of the 20th century, when it was
rediscovered. The crop has gained a relatively high degree of interest,
mainly due to high nutritional value of oils, obtained from its seeds
[1,2]. Several wholesome features, derived from the nutritional and
functional characteristics, made Chia considered as a food by the FDA
(Food and Drug Administration) and similarly, the European Commis-
sion authorized chia seeds as a novel food ingredient (2009/827/EC)
[2].

Abbreviations: FFAs, free fatty acids; GC, gas cromatography; AARD, average absolute relative deviations; CO2, carbon dioxide
⁎
Corresponding author.
E-mail address: masa.knez@um.si (M. Knez Hrnčič).

https://doi.org/10.1016/j.supflu.2018.06.017
Received 25 May 2018; Received in revised form 22 June 2018; Accepted 23 June 2018
Available online 25 June 2018
0896-8446/ © 2018 Elsevier B.V. All rights reserved.
M. Knez Hrnčič et al. The Journal of Supercritical Fluids 140 (2018) 182–187

The plant produces black and white seeds. Chia seeds are generally Table 1
small, approximately 2 mm long, 1–1.5 mm wide and thicker than PhysicochemicalPropertiesa of fluid [23].
1.0 mm, flat and oval shaped. Black colored chia seeds, which are more Fluid Tc / °C Pc / bar ω 1030 μ/C m
common, only slightly differ from the white seeds by their morphology;
white seeds are larger, thicker and broader than the black seeds. Their n-propane (C3H8) 96.65 42.5 0.152 0.280
composition is similar, it is reported that the average moisture content a
Tc, critical temperature; Pc, critical pressure; ω, accentric factor; μ, dipole
of black and white seeds is around 6%, one third of the material is the
moment.
oil, however, some authors report deviations in protein and fatty acid
composition of both seed varieties [3,4].
in order to optimize process parameters. Extraction kinetics of super-
In human nutrition, Chia seeds can be used as whole, milled or
critical extraction processes have been widely studied in order to de-
ground. Oil extracted from chia seeds can also be used in food [4,5]
velop optimal extraction models [15–19]. These models can easily be
Recently, several evaluations of chia's properties and possible uses
applied to several supercritical extraction processes with very high
have been performed. The studies have shown a high content of oil,
accuracy.
from 30 to more than 40%, of which 60% represents (omega) ω-3 al-
Extraction techniques using supercritical fluids have great ad-
phalinolenic acid and 20% (omega) ω-6 linoleic acid [6]. Both essential
vantages over conventional processes due to the lower operating tem-
fatty acids are associated with various benefits to consumer health,
peratures (suitable for thermolabile fatty acids), absence of organic
including is known to act on the prevention of cardiovascular diseases,
solvents in the final product (concentrated high quality product), no
decreasing the risk of heart and other chronic diseases such as type 2
need for further treatment of extract solution (absence of high eva-
diabetes and cancer, and protecting against Alzheimer’s [7].
poration temperatures), beneficial environmental impact due to re-
Chia crop has certainly a high potential to become a part of a
duced use of solvents in the production process and at industrial scale,
modern balanced diet, not only because of its oil quality, but also due to
batch consistency and compliance with regulatory requirements
the presence of natural antioxidants, protein (15–20%), carbohydrates
(quality assurance). Supercritical fluid extraction yields extracts free of
(26–41%), high dietary fibre (18–30%), ash (4–5%), minerals, vitamins,
solvent residues. The obtained products need no further purification in
and dry matter (90–93%). Since Chia is identified as a species with oil
sense of solvent elimination. Supercritical CO2 as well as propane are
production potential, many oil extraction methods had been utilized.
affordable solvents. Product recovery is accomplished via a simple
Variations in the extraction conditions, method and solvent choice re-
pressure reduction and compounds in a complex mixture can be se-
sulted in differences in the oil yield, quality of fatty acids, fatty acid
lectively separated using the pressure dependent dissolving power of
contents, total dietary fibres, and also antioxidant content. Oil extrac-
supercritical fluids. Lesser operating costs are commonly realized since
tion of Chia, however, produces a subfraction with relatively high
compression energy is more effective than distillation energy.
dietary fibre content rich on polyphenols, possibly involved in high
In the present study, Salvia hispanica L. oils have been extracted by
antioxidant activity, and compounds conferring functional character-
subcritical n-propane at two different temperatures, 40 °C and 60 °C.
istics with food system applications [8].
The operating pressure has been elevated up to 300 bar in order to
Extraction of oil from chia seed has been traditionally performed by
compare the extraction yield and composition of the extracts with the
cold pressing technique. This method is certainly featured by better
available literature data [20] and to verify the aim of obtaining higher
preservation of antioxidant contents such as quercetin and myricetin
extraction yields at higher pressures and/or temperatures than the ones
than solvent extraction [4]. However, recovery of oil yield is relatively
utilized in the previous studies [20]. Two sets of experiments at the
low [3]. Amongst solvent extraction techniques, Soxhlet method using
same processing conditions have been performed by subjecting the
n-hexane has been most widely applied despite it is less preferable than
black and white color seeds to the extraction process. Influence of ex-
other methods, which do not involve aggressive organic solvents [9].
traction conditions and material type on the extraction kinetics has
Soxhlet extraction yields in oil with a high absorption capacity, organic
been experimentally determined and the results were fitted to the mass
molecule absorption, and emulsifying stability. As the main dis-
– transfer model purposed by Brunner [16]. The composition of ob-
advantage, such products, which may contain traces of solvent are not
tained oils was determined via gas chromatography. The concentration
suitable for applications in food industry and other branches, producing
of key compounds omega-3and omega-6 was compared in the extracts
valuable products for human use. Besides, a slight loss of antioxidant
obtained by subcritical extraction with n-propane and extracts obtained
content has been noticed. Modern extraction techniques, such as pres-
with Soxhlet and ultrasonic extraction using n-hexane. The objective of
surized liquid extraction based on green chemistry solvents, are being
this work was to evaluate the extraction yield and the quality of oil
developed as an alternative to traditional methods for oil extraction
extracted from chia seeds with different extraction methods. An influ-
[10]. Chia oil obtained by ultrasound-assisted extraction using ethyl
ence of elevated operating pressures i.e. (100 bar, 200 bar and 300 bar)
acetate as solvent demonstrated high content of FFAs [11,12]. Super-
and temperature (40 °C and 60 °C) on the extraction yield and extract
critical fluid extraction represents a promising alternative extraction
composition is presented. Additionally, the comparison between dif-
method, especially due to the minor degradation of the bioactive
ferent extraction methods is given. For an extended evaluation, the cold
components. CO2 and n-propane are most frequently used as solvents,
pressing of Chia seeds was carried out. This study demonstrates that the
since preserving oil quality characteristics and selective extraction of
use of propane as extraction solvent allows the production of solvent-
free lipids from toxic residues. Uribe et al. and Ixtaina et al. have al-
free extracts rich on essential fatty acids.
ready preformed oil extraction from Chia seeds using supercritical CO2
up to 400 bar and temperatures from 40 °C to 80 °C as a good alter-
native because due to achieve a chia oil satisfactory yield with a similar 2. Materials and methods
fatty acid composition using an environmentally friendly process
[13,14]. 2.1. Chemicals
However, n-propane has been demonstrated as a better alternative
than CO2 for oil extraction, due to its non-polarity (Table 1) and con- Two types of Chia seeds (Chia seed hispanica black and Chia seed
sequent high solvent power for lipids. hispanica white) were supplied by Afred Galke GmbH (Samtgemeinde
Design of the extraction plant is certainly a complicated procedure, Bad Grund, Germany). N-propane used for subcritical fluid extraction of
which requires knowledge of phase equilibria and the knowledge of 99.5% w/w% purity was supplied by Linde (Celje, Slovenia). Fatty
mass transfer rates, determined by the time needed for the extraction. acids standards (palmitic acid, palmitoleic acid, oleic acid, stearic acid,
Therefore, it is highly recommended to calculate the extraction process linolenic acid, linoleic acid for GC analysis (purity 99.9%) were

183
M. Knez Hrnčič et al.
Fig. 1. Apparatus for high pressure extraction. 1, n-propane reservoir; 2, high pressure pump; 3, one-way valve; 4, heating coil; 5, extractor; 6, thermo bath; 7,
temperature indicator and regulator; 8, manometer; 9, sampling trap; 10, flow-meter.
purchased form Sigma Aldrich Chemie (Buchs, Switzerland).
2.2. Subcritical fluid extraction (SFE)
Chia seeds were extracted using subcritical n-propane in a semi-
continuous high-pressure flow-up apparatus. The procedure of lab-scale
extraction process is already described in a previous research [21] and
is shown in Fig. 1.
Extractions were carried out in cycles at pressures of 100 bar,
200 bar and 300 bar and temperatures of 40 °C and 60 °C. Firstly 10 g of
milled material (d = 0.05 mm) was filled into the extractor. After the
setting the temperature n-propane was pumped into the extractor and
extract was collected in a glass trap at atmospheric conditions. The flow
rate of n-propane was around 0.12 kg/h and was determined by the gas
flow meter.
2.3. Conventional solvent extraction methods
2.3.1. Soxhlet extraction
The Soxhlet extraction was performed using n-hexane as a solvent.
20 g of minced material was introduced into tube and 200 mL of solvent
was added into flask. Extraction was carried out in cycles for approxi-
mately 3 h at the boiling point of the solvent. Afterwards the solvent
was evaporated, and yield was calculated.
2.3.2. Ultrasonic extraction
Milled chia seed (20 g) was introduced to a 250 ml erlenmeyer flask
and 200 mL of n-hexane was added. Then the erlenmeyer flask was
immersed into an ultrasonic bath (40 kHz) with the liquid level in the
erlenmeyer flask kept lower than that of the bath. Extraction was per-
formed at constant temperature of 25 °C for 1 h. Than the mixture was
filtered and solvent evaporated. Extraction yield was calculated.
2.4. Cold pressing
The seeds were cold pressed using screw press (Model CA 59G, IBG
Monforts, Mönchengladbach) The oil content was gravimetrically de-
termined and expressed as weight percentage on dry basis (%, d.b.).
2.5. Modelling
The extraction curves off Chia oil were adjusted using mathematical
model proposed by Brunner, usually employed to model extraction ki-
netic curves obtained in the pilot-scale extraction apparatus. Brunner’s
equation is simple and can be used for many processes [16]. In our
work a modified equation (Eq. (2.1)) was used:
YE = x 0 (1−e−k ∙ f ) (2.1)
Where YE means yield of extraction (%), x 0 is extraction yield (%), k is a
constant and f is the solvent to feed ratio (kg of n-propane/kg of dried
material) during the process. The parameters were calculated using
184
The Journal of Supercritical Fluids 140 (2018) 182–187
non-linear regression method.
2.6. Analytical method for determination of free fatty acids (FFAs)
For determination of FFAs gas chromatography GC with FID de-
tector was used. First the FFAs were prepared using saponification
method described in previous research by Kotnik et al. [22]. Briefly the
NaOH solution was prepared dissolving 24 g NaOH and 0.25 g in 80 mL
water then 80 mL of ethanol was added. To 1 g of chia oil 2 mL of
prepared NaOH solution was added and afterwards heated to 60 °C and
stirred for 1 h at 550 rpm. Next the 0.4 mL of water and 4 mL of n-
hexane was add. The solution was stirred at room temperature for 1 h.
Then the upper layer was removed and to lower layer 1.6 mL of water
was added. Afterward 12 N hydrochloric acid was added to the mixture
to pH 1. The obtained upper layer containing FFAs was dried with
anhydrous MgSO4 and solvent was evaporated on a vacuum rotary
evaporator.
The analyses were performed for palmitic, palmitoleic, stearic,
oleic, linoleic and linoleic acids. GC model 2010 Shimadzu (Japan) with
column (HP-FFAP 30 m × 0.25 mm × 0.25 μm) and FID temperature
set at 300 °C was used. The oven time–temperature profile was as fol-
lows 120 °C (1 min), 25 °C/min–180 °C (1 min), 5 °C/min–220 °C
(10 min), 5 °C/min–230 °C (30 min). The carrier gas was helium with
total flow through the column 44.0 mL/min and split was 50. The
samples were analysed in n-hexane solutions. The quantification of FFA
was made using individual calibration curves. Each data point was
measured at least three times.
3. Results and discussion
3.1. Extraction yield
Effect of pressure and temperature on the extraction kinetic curves
at each experimental condition are presented in Figs. 2 and 3 as a
function of the propane quantity which was employed in the processes
for both materials. It is evident that higher operating pressure gave
higher extraction yields in the case of higher operating temperature. At
the same time, there are no significant differences in overall extraction
yields when both different seed varieties to the same operating condi-
tions. Higher temperature resulted in a higher extraction yield at a
constant pressure of 100 bar and 200 bar, while at the pressure of
300 bar the impact of operating temperature on the extraction yield was
negligible.
For White chia seeds, at a constant temperature of 40 °C, influence
of pressure was barely noticed. Extraction yield was only slightly de-
creased by increasing pressure from 100 bar to 200 bar; the total ex-
traction yield was somewhat lower than 18%, whilst at 300 bar, the
yield increased to about 20% (Fig. 2). As mentioned above, higher
operating temperature gave similar extraction yields at isochoric con-
ditions. The influence of pressure was much more significant. At 60 °C,
the total yield was about 20% at 100 bar; slightly higher than at the
M. Knez Hrnčič et al. The Journal of Supercritical Fluids 140 (2018) 182–187

Fig. 2. Comparative study between experimental data and Brunner’s extraction

model for White Chia seeds (100 bar–300 bar, 40 °C and 60 °C). Fig. 4. Diagram of extraction Yield [%] in dependence of density of propane
[kg m−3].

kinetics is low, extraction yields were similar at the temperature of

60 °C. Increasing pressure resulted in higher extraction yields, which
elevated from approximately 15% at 100 bar to almost 20% at 300 bar.
It is obvious that pressure is the key operating parameter that impacts
extraction kinetics most intensely. Impact of temperature is almost
negligible, as well as the type of material. This is clearly demonstrated
by the fact that extraction yields were similar for both materials,
maximal yield was about 20%, attained at highest operating pressures.
The highest yield was observed at 60 °C in the case of White chia seeds,
whilst at 40 °C for Black chia seeds. Compared to the literature data,
extraction yields are higher than those, reported after extraction with
carbon dioxide. Uribe and co-workers investigated impact of operating
conditions on the total extraction yield at pressures: 136 bar, 272 bar,
and 408 bar, and temperatures of 40 °C, 60 °C and 80 °C. Pressure has a
more significant effect than temperature on the extraction yield.
Fig. 3. Comparative study between experimental data and Brunner’s extraction Highest yield (7.18%) was reported at 408 bar and 80 ◦C [21].
model for Black Chia seeds (100 bar–300 bar, 40 °C and 60 °C). Extraction yield of Soxhlet extraction for Black and White chia was
18.4% and 14% respectively. For ultrasonic extraction yield was fairly
lower operating temperature, similar yield has been attained at 200 bar. lower; 16.7% for Black and 13.4% for White chia seeds. Yield of cold
The total yield increased above 20% at the highest operating pressure. pressing was the lowest, for Black and White chia was 15.4% and 12.3%
This was also the highest extraction yield that was attained. Experi- respectively.
mentally obtained extraction yields were compared with those from a
study by Zanqui et al. In that experiments, the maximum pressure was 3.2. Kinetic model
120 bar. Maximum extraction yield was 28.16% at the temperature of
45 °C and pressure 100 bar, which not consistent with the data obtained Using Brunner’s method results were fitted to the Brunner’s mass
in this study, assuming higher solubility of fatty acids in a denser ex- transfer model, obtaining a minor deviation of experimentally de-
traction medium. According to the results obtained by Zanqui et. al and termined kinetic curves from the mathematical model.
co-workers, pressure has almost no impact on the extraction yield, Brunner’s model parameters are presented in Table 2 and correla-
however experiments have been performed in a narrower pressure tion between the model and the experimental data is shown in Figs. 2
range. Anyhow, at a constant temperature, increasing the pressure in- and 3. Most of the curves fit almost completely to the model in the
creases the density of propane and consequently its solvent strength entire operating range. Slight deviations may be observed in case of the
thus increases the solubility of fatty acids. Likewise, for Black chia curves attained at 40 °C at 100 bar and 200 bar. At 60 °C,
seeds, increasing pressure contributed to the higher extraction yield
isothermal operating conditions. At the temperature of 40 °C, the total Table 2
yield increased from 14.3% at 100 bar up to almost 20.4% at 300 bar. Calculated parameters of the Brunner model for Chia seeds extraction.
This conclusion fits well to the fact that increasing solvent density seeds p [bar] T [°C] k X0 AARD %
contributes to the higher solvent power of propane for fatty acids;
namely at 40 °C propane density is about 495 kg/m3 at 100 bar and White Chia 100 40 0.2711 17.25 3.13
60 0.3302 17.92 3.66
532.22 kg/m3 at 300 bar (Fig. 3). Our results suggest that the solubility
200 40 0.3802 16.31 6.54
of fatty acids in propane is proportional to the density of propane. An 60 0.3198 18.92 4.11
evident relationship between the solvent density and extraction yield 300 40 0.2580 19.34 4.50
has been observed (Fig. 4) for both materials. The slopes of the curves 60 0.6129 19.17 4.49
Black Chia 100 40 0.2309 13.45 5.43
are relatively soft for density range up to 490 kg/m3, but become
60 0.1626 14.62 1.87
steeper as solvent density increases up to 500 kg/m3 in case of White 200 40 0.2119 16.05 7.27
chia seeds. Almost a linear relationship between solvent density and 60 0.1524 17.24 3.65
extraction yield may be considered for the black seeds. 300 40 0.3089 19.17 3.92
As mentioned above, impact of extraction temperature on the 60 0.2296 18.35 3.63

185
M. Knez Hrnčič et al. The Journal of Supercritical Fluids 140 (2018) 182–187

Table 3
GC analysis of free fatty acids from extracted Chia seeds.
FFA
[%]

conditions Palmitic Stearic Oleic Linoleic Linolenic

(ω-6) (ω -3)

White 100 bar – 40 °C 8.20 ± 0.09 7.89 ± 0.07 10.17 ± 0.09 20.04 ± 0.05 53.67 ± 0.08
Chia 100 bar – 60 °C 8.03 ± 0.09 6.39 ± 0.03 9.18 ± 0.07 19.80 ± 0.12 56.60 ± 0.09
200 bar – 40 °C 8.05 ± 0.08 6.61 ± 0.05 9.26 ± 0.06 19.97 ± 0.25 56.11 ± 0.11
200 bar – 60 °C 7.83 ± 0.07 6.19 ± 0.06 9.00 ± 0.07 19.55 ± 0.04 57.42 ± 0.08
300 bar – 40 °C 7.69 ± 0.07 6.50 ± 0.02 9.42 ± 0.05 19.81 ± 0.06 56.58 ± 0.05
300 bar – 60 °C 7.90 ± 0.05 6.10 ± 0.04 8.97 ± 0.04 20.11 ± 0.09 56.92 ± 0.18
Black 100 bar – 40 °C 7.54 ± 0.07 6.00 ± 0.04 8.03 ± 0.06 19.23 ± 0.06 59.20 ± 0.09
Chia 100 bar – 60 °C 7.48 ± 0.06 5.93 ± 0.07 7.98 ± 0.07 19.46 ± 0.32 59.15 ± 0.12
200 bar – 40 °C 7.50 ± 0.03 5.76 ± 0.03 7.75 ± 0.07 19.49 ± 0.28 59.50 ± 0.29
200 bar – 60 °C 7.69 ± 0.08 5.67 ± 0.05 7.77 ± 0.09 19.80 ± 0.06 59.06 ± 0.07
300 bar – 40 °C 7.46 ± 0.06 5.60 ± 0.05 7.74 ± 0.07 19.47 ± 0.08 59.73 ± 0.11
300 bar – 60 °C 7.50 ± 0.06 5.83 ± 0.04 7.91 ± 0.07 19.47 ± 0.05 59.29 ± 0.06

experimentally measured values for white seeds are higher than the
ones calculated using the model at 300 bar. For those curves, better
fitting is observed at lower S/F ratios, where the samples have been
taken every five minutes. With increasing S/F ratio, the discrepancy
becomes greater. According to the model, the yield is almost constant
after S/F ratio reaches the value of 15–20 kg of propane per kg of dry
material. Based on our results, the yield is still growing, but however,
with a lower increment. Similar conclusions can be done for both ma-
terials, independently on extraction conditions. The average absolute
relative deviations (AARD) between experimental and calculated data is
in range from 3.13% to 7.27% and is presented in Table 2.

3.3. Analysis of chia extract

The content of FFAs of Chia extract is presented in Table 3 for
propane extracts and Table 4 for n-hexane extracts. An example of fatty
acids profile of Chia seed extract obtained by gas chromatography
analysis is presented on Fig. 5.
GC analyses were performed for palmitic, palmitoleic, stearic, oleic,
linoleic and linolenic acids, but presence of palmitoleic acid has not
been demonstrated. From the results can be seen that Chia seeds are
generally rich with ω-3 and ω-6 acids. The differences in the content in
each propane extract are minimal, however, the content of palmitic,
stearic, oleic and linoleic acids is higher in extracts, attained from
White Chia seeds, whilst the content of linolenic acid was higher in
black seed extracts. The major compound identified in all oils was li-
nolenic acid. In propane extracts, the content of linolenic acid was the
highest (almost 60%), followed by linoleic acid (around 20%), oleic
(10%), the content of stearic and palmitic acid is lower than 10% each.
These FFAs occur in a similar percentage, independently on operating
pressures and temperatures. On the contrary, the content of linolenic
acid, which was also higher in black seed extracts, increased with
Fig. 5. Profile of fatty acids from Chia extract obtained with gas chromato-
graphy analysis: 1 – palmitic, 2 – stearic, 3 – oleic, 4 – linoleic, 5 – linolenic.
increasing operating pressure. The influence of temperature is almost
imperceptible, except for White chia seed extracts, attained at lower
operating pressures, where the elevation of temperature increased the
content of the linolenic acid for almost 3%. The content of linolenic acid
was generally by far the highest and also most affected by changing
operating conditions, almost 57% in white seed extracts attained at
300 bar and 60 °C and 59.73% in extracts, obtained from black seeds
300 bar and 40 °C. Despite this fact, at equal pressures, generally the
percentage of the free fatty acids within the extract was higher at higher
temperatures, the most probable explanation is that they were more
easily dissolved by the solvent.
GC analysis of free fatty acids from Chia seeds attained with Soxhlet
and ultrasonic extraction and from cold-pressed seeds are presented in
Table 4. Compositions of the oils obtained by conventional solvent

Table 4
GC analysis of free fatty acids from Chia seeds extracts obtained with Soxhlet and ultrasonic extraction and cold-pressed seeds.
FFA
[%]

Type Palmitic Stearic Oleic Linoleic Linolenic

(ω-6) (ω-6) (ω -3)

a
White Cold-pressed 11.22 ± 0.11 11.01 ± 0.10 10.60 ± 0.12 19.78 ± 0.09 47.34 ± 0.09
Chia Soxhlet 10.55 ± 0.13 10.47 ± 0.13 10.95 ± 0.09 17.98 ± 0.12 48.52 ± 0.13
Ultrasonic 9.74 ± 0.08 8.63 ± 0.08 10.01 ± 0.10 19.51 ± 0.25 51.53 ± 0.11
Black Cold-pressed 14.82 ± 0.11 12.62 ± 0.21 8.88 ± 0.09 17.53 ± 0.11 46.15 ± 0.18
Chia Soxhlet 12.72 ± 0.12 11.64 ± 0.17 9.00 ± 0.13 17.98 ± 0.08 48.66 ± 0.16
Ultrasonic 12.17 ± 0.26 11.93 ± 0.11 9.97 ± 0.08 19.51 ± 0.15 46.43 ± 0.09

a
Percentage standard deviation.

186
M. Knez Hrnčič et al.
extraction methods slightly differ from those of propane extracts. The
calculated percentage of oleic, stearic and palmitic acids in extracts
obtained with hexane was higher than in extracts obtained with pro-
pane, it may be because the content of polyunsaturated acids in extract
was lower and not because the content of the three acids was higher.
The lower content of linoleic acid and particularly linolenic acid could
be related to degradation of these labile substances. Yet again, linolenic
acid was present in the largest proportion (about 50%), followed by
linoleic acid; around 18% in Soxhlet extracts and cold press oil, and
whilst in ultrasonic extracts the content was almost 20%.
4. Conclusion
To accomplish, extraction yield and composition of extracts from
Chia seeds are slightly affected by the different process parameters
studied (pressure, temperature). Additionally, it has been demonstrated
that the composition of both, Black and White chia seed extract is si-
milar. The use of different extraction conditions resulted in differing
extraction yields, but did not significantly affect the composition of
extract. Higher operating pressures contributed to higher extraction
yields when operating at higher temperature. It has been demonstrated,
that the composition of oils, obtained from both seed varieties is similar
and is comparable to the data available in the literature [13,14,20].
Brunner’s equation was employed to model extraction kinetic curves
which were obtained in the lab-scale extraction apparatus. The accu-
racy of the model with experimental data has been proven. The
agreement between experimental and model data was from 3.13% to
7.27%.
GC analyses confirmed presence of palmitic, stearic, oleic, linoleic
and linoleic acids. Linolenic acid is represented in the highest amount
which increased with elevating operating pressure. Highest operating
pressures compared to the available literature data were examined in
the frame of the present research. Propane has been demonstrated as a
suitable processing media for extraction of oils with a high content of
the two essential fatty acids (α-linolenic acid and linoleic acid). It can
be concluded that high operating pressure contributes to the higher
extraction yield and the higher content of linolenic acid, the major
compound in the extracted oils. The results suggest that the subcritical
extraction with food grade n-propane is a potential method for ob-
taining high-quality chia seed oil, providing a product free of toxic
residues, and therefore, suitable for subsequent use in food, pharma-
ceutical, and cosmetic industries.
Technologies with sub- and supercritical fluids have low environ-
mental impact and beneficially contribute to the human health and the
quality of life. Propane can be considered as a appropriate solvent for
isolation of oils with antioxidant and pharmacological properties with a
high proportion of bioactive compounds including fatty acids from the
seeds. The synergistic effect of extracts result in anti-tumor, antioxidant
and antimutagenic potential. Often the isolated complexes exhibit
strong anti-microbial activity and may represent natural preservatives
for food and feed.
Acknowledgement
Special thanks to the Slovenian Research Agency (ARRS) for fi-
nancial support of research programme group P2 – 0046: Separation
processes and production design, contract No. 1000-15-0552.
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