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ABSTRACT Encapsulation of poly-unsaturated fatty acid (PUFA)is an alternative to increase its stability during processing and storage. Chia (Salvia hispanica L.) oil is a reliable source of both omega-3 and omega-6 and its encapsulation must be better evaluated as an effort to increase the number of foodstuffs containing PUFAs to consumers. In this work chia oil was extracted and encapsulated in stearic acid microparticles by the hot homogenization technique. UV-Vis spectroscopy coupled with Multivariate Curve Resolution with Alternating Least-Squares methodology demonstrated that no oil degradation or tocopherol loss occurred during heating. After lyophilization, the fatty acids profile of the oil-loaded microparticles was determined by gas chromatography and compared to in natura oil. Both omega-3 and omega-6 were effectively encapsulated, keeping the same omega-3:omega-6 ratio presented in the in natura oil. Calorimetric analysis confirmed that encapsulation improved the thermal stability of the chia oil.
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Vol. 34, No. 03, pp. 659 – 669, July – September, 2017
* To whom correspondence should be addressed
This is an extended version of the work presented at the
11th Brazilian Congress of Chemical Engineering on Undergraduate Scientic Mentorship, COBEQ-IC 2015
Campinas, SP, Brazil
M. F. Souza1, C. R. L.Francisco1; J. L. Sanchez2, A. Guimarães-Inácio2,
P. Valderrama2, E. Bona2, A. A. C. Tanamati1, F. V. Leimann2 and O. H. Gonçalves2*
1Universidade Tecnológica Federal do Paraná, Departamento de Alimentos, Via Rosalina Maria dos Santos, 1233,
Caixa Postal 271, 87301-899 Campo Mourão, PR, Brasil. Phone/Fax: +55 (44) 3518-1400
2Universidade Tecnológica Federal do Paraná, Programa de Pós-Graduação em Tecnologia de Alimentos, Via Rosalina Maria dos Santos,
1233, Caixa Postal 271, 87301-899 Campo Mourão, PR, Brasil. Phone/Fax: +55 (44) 3518-1400
(Submitted: October 14, 2015; Revised: August 25, 2016; Accepted: September 6, 2016)
ABSTRACT - Encapsulation of polyunsaturated fatty acid (PUFA)is an alternative to increase its stability during
processing and storage. Chia (Salvia hispanica L.) oil is a reliable source of both omega-3 and omega-6 and its
encapsulation must be better evaluated as an eort to increase the number of foodstus containing PUFAs to consumers.
In this work chia oil was extracted and encapsulated in stearic acid microparticles by the hot homogenization technique.
UV-Vis spectroscopy coupled with Multivariate Curve Resolution with Alternating Least-Squares methodology
demonstrated that no oil degradation or tocopherol loss occurred during heating. After lyophilization, the fatty acids
prole of the oil-loaded microparticles was determined by gas chromatography and compared to in natura oil. Both
omega-3 and omega-6 were eectively encapsulated, keeping the same omega-3:omega-6 ratio presented in the in
natura oil. Calorimetric analysis conrmed that encapsulation improved the thermal stability of the chia oil.
Keywords: encapsulation, polyunsaturated fatty acid, solid lipid microparticles, Salvia hispanica, MCR-ALS.
The increasing demand for functional foods has directed
the market towards oering omega3-enriched foodstu.
It is a modern lifestyle challenge to meet the required
amount of polyunsaturated fatty acids (PUFAs) in order to
minimize the risk of chronic disease (Garg et al., 2006).
Chia (Salvia hispanica L.) oil have high nutritional value
since most of its constituents are triglycerides with PUFA
acids present in larger proportions and omega-3 content
between 60 and 68% (Capitani et al., 2012). PUFAs are
known to help reduce triglycerides and cholesterol levels
and other benecial eects have been observed regarding
coronary heart disease, hypertension and inammatory
disorders(Borneo et al., 2007; Harris et al., 2008). Although
sh oil is a less expensive source of omega-3, its use in
food formulations has been questioned due to unpleasant
sensory properties even after encapsulation (Martínez et
al., 2012; Muchow et al., 2009; Rodea-González et al.,
PUFAs are susceptible to oxidation(Ixtaina et al.,
2011), which can lead to a decrease in nutritional and
sensory quality. Encapsulation techniques are a promising
approach in order to protect substances from harm and to
meet shelf-life requirements (Gökmen et al., 2011; Gouin,
2004). There are a number of encapsulation techniques to
encapsulate liquid lipids (TAMJIDI et al., 2013a) such as
spray drying (Carneiro et al., 2013; Jimenez et al., 2006;
Rodea-González et al., 2012), cyclodextrin complexation
(XU et al., 2013), complex coacervation (Tamujidi et al.,
2012) and ultrasonic atomization (Klaypradit; Huang,
Brazilian Journal
of Chemical
ISSN 0104-6632
Printed in Brazil
Brazilian Journal of Chemical Engineering
M. F. Souza, C. R. L.Francisco, J. L. Sanchez, A. Guimarães-Inácio,
P. Valderrama, E. Bona, A. A. C. Tanamati, F. V. Leimann and O. H. Gonçalves
2008). Borneo et al. (2007) obtained cream-lled sandwich
cookies containing encapsulated omega-3, demonstrating
the possibility of producing shelf-stable foods with
high levels of omega-3. Gökmen et al. (2011) observed
a reduction in the thermal oxidation of omega-3 from
axseed oil after its encapsulation. Rodea-González et al.
(2012) produced microparticles containing chia oil by spray
drying using whey protein concentrate-polysaccharide
Hot homogenization is also an interesting technique
due to the natural compatibility between PUFAs and
the solid lipid matrix (Lacatusu et al., 2013; Muchow et
al., 2009; Salminen et al., 2013). Encapsulation by hot
homogenization is also favored by the fact that the liquid
oil hinders the solid lipid crystallization, generating a
less ordered microstructure or even an amorphous phase
(Tamjidi et al., 2013b). Although no solvent is required,
relatively high temperatures are needed for the proper
mixing of encapsulant and the encapsulated compound.
For this reason, attention must be paid to the possibility
of thermal degradation when unsaturated lipids are to be
encapsulated. Oil degradation may be detected by UVVis
spectroscopy, but the complexity of the obtained spectra
requires further signal treatment. Multivariate Curve
Resolution (MCR) is a suitable chemometric technique
since it can identify mixed signals and recover the relative
concentration of the substances and their respective spectra
(Março et al., 2014).In the case of unsaturated fatty acids,
thermal degradation can be evaluated by the formation of
degradation products such as conjugated trienes and dienes
and hydrolysis products (Gonçalves et al., 2014).
Moreover, some key points are still to be investigated
in the encapsulation of chia oil by the hot homogenization
procedure. First, the encapsulation eciency of each
PUFA must be determined since it can be aected by the
interactions between them and the encapsulant. Second, the
possibility of thermal degradation must be checked since
the system must be heated during the particle production
step. The objective of this work was to extract the oil from
chia seeds and encapsulate it in stearic acid microparticles
by the hot homogenization technique. Multivariate Curve
Resolution (MCR) was applied to determine if damage to
the oil occurred due to heating. Encapsulation eciency
was determined for both omega-3 and omega-6 using gas
Chia seeds were acquired from the local market. Stearic
acid (Sigma-Aldrich, 99.5%) and Tween 80 (Dinâmica,
97%) were used as encapsulant and surfactant, respectively.
Distilled water was used as continuous phase. Methanol
(Isofar, 99.8%), chloroform (Vetec, 99.5%), ammonium
chloride (Vetec, 99.5%) and sulphuric acid (Vetec, 95%)
were used in the transesterication reaction. KBr (Sigma-
Aldrich, spectrophotometric standard) was used in the
spectrophotometric analyses.
Chia oil extraction
Total moisture of the chia seeds was determined and
then adjusted to 80% by adding distilled water. Then, the
extraction was performed according to the methodology
described by Bligh and Dyer (1959). Briey, triturated
chia seeds (15g) were added to methanol (30 mL) and
chloroform (15 mL) under mild stirring. Then, 15 mL
distilled water was added and stirred for another 5
minutes. The resulting solution was ltered and 20 mL
more chloroform was added. After 5 minutes stirring, the
solution was ltered again. Solvent was removed under
vacuum (-400 mmHg e 35ºC) and the chia oil was stored at
10°C protected from light.
Quantication of the degradation products by MCR-
Quantication of the oil degradation products
was carried out to determine if chia oil was prone to
degrade at the temperature used in the encapsulation
procedure (75°C). A sample of in natura chia oil (before
encapsulation) was heated and aliquots were collected at
28, 30, 40, 50, 60, 70 e 75ºC. The sample was then kept at
75ºC and additional aliquots were collected after regular
time intervals for 120 minutes. UV-Visible spectra (Ocean
Optics, Red Tide USB650, 1 nm resolution) were obtained
and the formation of degradation products was evaluated
by Multivariate Curve Resolution Alternating Least-
Squares method (MCR-ALS) as described by Gonçalves et
al.(2014). Spectra recovered by MCR-ALS were attributed
to their respective compounds according to Valderrama et
al. (2011).
Microparticles production
Chia oil-loaded microparticles were obtained by the
hot homogenization technique(Gonzalez-Mira et al., 2010)
such as non-steroidal anti-inammatory drugs (NSAIDs.
Aqueous phase was prepared dissolving Tween 80 (0.300
g) in distilled water (25 g) and heating to 75°C under
gentle stirring. Separately, stearic acid (0.625g) was melted
at 75°C in a borosilicate double walled vessel. Chia oil
was then added to the molten lipid and mixed for 1 minute.
Then, the aqueous phase was added to the vessel and stirred
for 3 minutes, resulting in an oil-in-water macroemulsion.
Sonication (Fisher-Scientic – Ultrasonic Dismembrator
120 W, 1/8” tip) was carried out for 3 minutes in a pulse
regime (30 seconds on and 10 seconds o). The sonicated
mixture was cooled in an ice bath, resulting in the
Brazilian Journal of Chemical Engineering Vol. 34, No. 03, pp. 659 – 669, July – September, 2017
Fatty acids prole of chia oil-loaded lipid microparticles 661
formation of solid lipid particles dispersed in water. They
were freeze dried before analysis. The same procedure was
also carried out without the addition of chia oil to obtain
blank microparticles.
Transesterication and Gas Chromatography (GC)
Fatty acids quantication was performed by CG using
methyl tricosanoate (23:0, Sigma-Aldrich) as internal
standard according to Hartman and Lago methodology
(Milinsk et al., 2008).Fatty acid methyl esters (FAMEs)
were separated and identied using chromatograph
standards (Sigma-Aldrich, F.A.M.E. Mix C14-C22).
The equipment setup was as follows: gas chromatograph
(Shimadzu, GC-2010 Plus AF) equipped with Split/
Splitless capillary injector, ame ionization detector
(FID), ow and pressure automatic controllers and a
100% dimethylpolysiloxane capillary column (Rtx-1,
30m x 0.25mm x 0.25µm). Transesterications were
performed in triplicate. Equation 1 was used in the FAMEs
quantication(Joseph and Ackman, 1992).
x CT
Mx= Fatty acid concentration in the sample (mg.g-1oil);
M23:0 = internal standard mass (mg);
Ms = sample mass (g);
AX = peak area for each fatty acid;
A23:0 = peak area of the internal standard;
FCT = theoretical correction factor;
FMEA = conversion factor.
Microparticles characterization
Fourier transform infrared spectroscopy (FTIR) was
used to qualitatively evaluate chia oil encapsulation.
Lyophilized samples or in natura oil were mixed with
dry KBr and spectra were acquired in a Shimadzu
spectrometer (IR Anity-1, 32 cumulative scans) from
4000 to 400 cm-1.This procedure was carried out in
triplicate. Images from the microparticles were taken using
an optical microscope (BIOVAL, L2000A) coupled to a
digital camera. Dierential Scanning Calorimetry (DSC,
Perkin Elmer 4000) was used to investigate the thermal
behavior of in natura chia oil, oil-loaded microcapsules
and blank microcapsules. In the rst set of experiments,
approximately 5 mg of samples were placed on open
aluminum lids and heated from 0°C to 440°C at 20°C/min
under air atmosphere (100 mL/min) in order to investigate
if encapsulation inuenced the thermal stability of the
chia oil. In a second set of experiments, approximately 5
mg of samples were placed on closed aluminum lids and
heated from 0°C to 250°C at 20°C/min under a nitrogen
atmosphere (10 mL/min) to determine the enthalpy of
fusion and melting temperature of the encapsulant.
To determine encapsulation eciency (EE%,
Equation 2), an aliquot of the microparticles dispersion
was ltered in Amicon lters (100 kDa, Millipore) using
an ultracentrifuge at 14,500 rpm for 15 min. The liquid
phase containing the non-encapsulated fatty acids ([FA]
non-encapsulated) was transesteried as described above.
Also, the total concentration of fatty acids ([FA]total,
encapsulated plus non-encapsulated) was determined for
the lyophilized microparticles.
( )
% 100
total non encapsulated
 
 
Chia oil composition
Chia seeds presented 9.5% humidity, which is in
accordance with values found in the literature (Ixtaina et
al., 2011). Total lipid content was 19.80%, while values
from 20.30 to 33.60% were reported when hot hexane or
pressing were used for extraction (Ixtaina et al., 2011). It
is worth noting that Bligh-Dyer (Bligh and Dyer, 1959)
is a cold method thus minimizing lipid oxidation during
Thermal degradation of in natura chia oil by MCR-
Figure1 presents the relative concentration of
tocopherol and degradation products (conjugated dienes/
trienes and hydrolysis products) for the in natura chia oil
(before its encapsulation) during heating to 75°C then
keeping at this temperature for 2 hours. In Figure 2, UV-
Vis spectra recovered by MCR-ALS of tocopherol and
degradation products are presented.
It is worth noting that the concern about thermal
degradation arises from the fact that the encapsulation
procedure demands heating to melt the lipid encapsulant,
which could damage the unsaturated fatty acids present
in chia oil. UV-Vis spectra detected the presence of
tocopherol (Ixtaina et al., 2011) and that its concentration
started decreasing only after approximately 2 hours at
75°C. Hydrolysis products were also formed after this
heating time. Gonçalves et al. (2014) have demonstrated
that temperature and oil composition are key factors for
tocopherol concentration decrease and oil degradation for
Brazilian Journal of Chemical Engineering
M. F. Souza, C. R. L.Francisco, J. L. Sanchez, A. Guimarães-Inácio,
P. Valderrama, E. Bona, A. A. C. Tanamati, F. V. Leimann and O. H. Gonçalves
a number of dierent edible oils. During the encapsulation
procedure adopted in this work, oil is heated at 75°C for
only 7 minutes, meaning that one may not expect chia oil
degradation caused by the encapsulation conditions (time
and temperature).
Figure 1. Relative concentration proles of tocopherol (—) and conjugated dienes/trienes and hydrolysis products (- - - -) for in natura chia
oil (before encapsulation) (A) in dierent temperatures and (B) at 75°C for 2 hours.
Figure 2. UV-Vis spectra recovered by MCR-ALS of (- - - -) tocopherol and (——) conjugated dienes/trienes and hydrolysis products.
Fatty acids identication and quantication
Figure 3 presents the separation of the fatty acids methyl
esters of the in natura chia oil before its encapsulation,
while the concentration (mg.g-1) of each compound is
presented in Table 1.
The most concentrated fatty acids found were palmitic
(C16:0, 67.88 mg.g-1), oleic (C18:1n-9, 54.09 mg.g-
1), linoleic (LA, 18:2n-6, omega 6, 181.94 mg.g-1) and
alpha-linolenic (LNA, 18:3n-3, omega-3, 565.52 mg.g-1).
Linoleic and alpha-linolenic essential fatty acids (LA e
LNA) were identied at 12 and 14 minutes, respectively
and corresponded to 20.21% and 62.80% of the total lipid
in chia oil. These results are in accordance with those
presented by Capitani et al. (2012)and Martínez et al.
Edible oils presenting a ΣPUFA:ΣSFA ratio above 0.45
and n-6:n-3 ratio from 1:1 to 2:1 are recognized as ideal to
human dietary intake (Wood et al., 2004), meaning that the
oil presented high nutritional quality.
Brazilian Journal of Chemical Engineering Vol. 34, No. 03, pp. 659 – 669, July – September, 2017
Fatty acids pro le of chia oil-loaded lipid microparticles 663
Figure 3. In natura chia oil chromatogram (before encapsulation).
Table 1. Fatty acids concentration in in natura chia oil (before encapsulation).
Fatty acid Concentration (mg.goil-1)
C14:0 (myristic acid) 0.32 ± 0.01
C16:0 (palmitic acid) 67.88 ± 1.75
C18:0 (stearic acid) 27.91 ± 0.73
C18:1 n-9 (oleic acid) 54.09 ± 1.36
C18:2 n-6 (linoleic acid) 181.94 ± 5.75
C18:3 n-3 (α linolenic acid) 565.52 ± 24.4
C20:0 (arachidic acid) 2.35 ± 0.04
C22:0 (behenic acid) 0.78 ± 0.03
Ratios and sums*
ΣSFA 99.24
ΣMUFA 54.09
ΣPUFA 747.46
n-6:n-3 0.32
*ΣSFA = saturated fatty acids; ΣMIFA = monounsaturated fatty acids; ΣPIFA = polyunsaturated fatty acids.
Chia oil-loaded particles were lyophilized and the
powder was transesteri ed and compared to in natura oil
(Figure 4). Also, non-encapsulated oil was separated from
the particles by ltration and subjected to transesteri cation
(Figure 5). Encapsulation e ciency (EE%) of omega-3
and omega-6 are presented in Table 2.
Brazilian Journal of Chemical Engineering
M. F. Souza, C. R. L.Francisco, J. L. Sanchez, A. Guimarães-Inácio,
P. Valderrama, E. Bona, A. A. C. Tanamati, F. V. Leimann and O. H. Gonçalves
Figure 4. Chromatograms of in natura chia oil (red) and oil-loaded particle (black).
Figure 5. Chromatograms of non-encapsulated chia oil (red) and oil–loaded particles (black).
Brazilian Journal of Chemical Engineering Vol. 34, No. 03, pp. 659 – 669, July – September, 2017
Fatty acids prole of chia oil-loaded lipid microparticles 665
Table 2. Fatty acids concentration of the chia oil-loaded microcapsules and the non-encapsulated oil.
Concentration (mgFA/gparticles)
Fatty acid Oil-loaded microcapsules Non encapsulated oil
C14:0 (myristic acid) 13.24 ± 0.15 0.84 ± 0.15
C16:0 (palmitic acid) 165.07 ± 64.91 23.67 ± 1.96
C18:0 (stearic acid) 682.17 ± 213.04 24.35 ± 7.35
C18:1 n-9 (oleic acid) 90.67 ± 0.80 21.51 ± 5.09
C18:2 n-6 (linoleic acid) 124.01 ± 0.19 9.57 ± 2.37
C18:3 n-3 (α linolenic acid) 388.71 ± 17.04 18.11 ± 3.29
C20:0 (arachidic acid) 7.35 ± 0.28 -
C22:0 (behenic acid) 1.34 ± 0.72 -
Ratios and sums*
ΣSFA 869.17 48.86
ΣMUFA 90.67 21.51
ΣPUFA 512. 72 27.68
ΣPUFA:ΣSFA 0.60 0.57
n-6:n-3 0.32 0.53
*ΣSFA = saturated fatty acids; ΣMIFA = monounsaturated fatty acids; ΣPIFA = polyunsaturated fatty acids.
Table 3. Encapsulation eciency (EE%) of omega-3 and omega-6.
Fatty acid Encapsulation
eciency (EE%)
C18:3 n-3
(omega-3) 95.4 ± 0.6
C18:2 n-6
(omega-6) 92.3 ± 1.9
Omega-3 and -6 peaks can be found in the microparticles
but in less intensity when compared to in natura oil because
particles are composed of the encapsulant (stearic acid) and
oil in 1:1 (m:m) proportion. Unidentied peaks can also
be observed, probably related to impurities in the stearic
acid. No signicant dierence between encapsulation of
omega-3 and omega-6 could be found (p>0.05), which
means that the omega-3:omega-6 ratio in the particles
and in in natura oil is statistically the same (3.14 ± 0.14
and 3.11 ± 0.05, respectively). This is important since
an imbalance of the omega6:omega3 ratio as presented
by modern Western food intake is related to a number of
chronic diseases and metabolic disorders (Simopoulos,
2008). These results demonstrate that the encapsulated oil
presents the same proportion of in natura chia oil, meaning
that the microcapsules may be used to protect the oil and to
formulate products with high nutritional value.
The literature reports typical encapsulation eciency
values for omega-3 and -6 from 70 to 80% (Rodea-González
et al., 2012), 57.2 to 89.6% (Jimenez et al., 2006), 62.3
to95.7% (Carneiro et al., 2013) and 45.8% to 58% (Xu et al.,
2013), depending on the encapsulant and the encapsulation
technique. Solid lipid nano or microparticle systems are
often suitable for oil encapsulation due to the compatibility
between the oil and the encapsulant matrix. Lacatusu et al.
(2013) encapsulated sh oil in nanostructured lipid carriers
with 88.5% eciency. Unfortunately some works in the
literature did not present information on eciency values,
possibly assuming total encapsulation (Muchow et al.,
2009; Salminen et al., 2013).
Particles characterization
Optical microscopy images of chia oil-loaded particles
and blank particles (no oil added) are presented in Figures
6 and 7, respectively. Figure 8 presents infrared spectra
of in natura chia oil, chia oil-loaded particles and blank
particles. All spectra were normalized in order to allow
comparison. Figure 9 (a) presents the DSC thermograms of
the chia oil-loaded microparticles and blank microparticles
(no oil added) under nitrogen atmosphere. In Figure 9 (b)
thermograms of chia oil and chia oil-loaded microparticles
under air atmosphere are presented.
Brazilian Journal of Chemical Engineering
M. F. Souza, C. R. L.Francisco, J. L. Sanchez, A. Guimarães-Inácio,
P. Valderrama, E. Bona, A. A. C. Tanamati, F. V. Leimann and O. H. Gonçalves
Figure 6. Optical microscopy image of blank microparticles (no chia oil added).
Figure 7. Optical microscopy image of chia oil-loaded microparticles
Absorption band at 3010 cm-1 associated to =C-H
groups was found at the chia oil spectrum as expected
(Vidal et al., 2013). Blank particles did not show this
band since stearic acid did not present any unsaturation
on its chemical structure. This band was also present at
the oil-loaded particles but in a much lower intensity. The
decrease in intensity could be an indication of ecient
entrapment of encapsulated compounds, also corroborating
the previously results found (optical microscopy and gas
Brazilian Journal of Chemical Engineering Vol. 34, No. 03, pp. 659 – 669, July – September, 2017
Fatty acids pro le of chia oil-loaded lipid microparticles 667
In natura (before encapsulation) chia oil begins
oxidation at approximately 145°C. Grampone et al. (2013)
reported an oxidation temperature of 176°C using pure
oxygen as oxidizing atmosphere at a higher rate.This
could explain the di erence, along with discrepancies
in oil composition, as the omega-6 concentration is not
reported by the authors. The same may be concluded when
comparing to the results from Ixtaina et al. (2012), who
reported an oxidation temperature of (168.2 ± 2.8)°C. DSC
thermograms demonstrated that the encapsulation of chia
oil increased its oxidative stability since oxidation began at
approximately 259°C. This behavior was also described in
the encapsulation of oregano oil in chitosan nanoparticles
(Hosseini et al., 2013), eugenol (Woranuch and Yoksan,
2013) and also carvacrol (Keawchaoon and Yoksan, 2011)
using thermogravimetric analysis.
Chia oil was extracted by using the Bligh-Dyer method
to minimize oil degradation during extraction. UV-Vis
spectroscopy coupled to multivariate analysis (MCR-
ALS) demonstrated that no oil degradation or tocopherol
loss were expected to occur under the experimental
conditions (heating time and temperature) applied in the
hot homogenization procedure used in this work. Chia oil
wase ciently encapsulated in micrometric stearic acid
particles as demonstrated bygas chromatography, UV-Vis,
DSC and FTIR spectroscopy. Encapsulation e ciencies for
omega3 and omega6 were similar, meaning that the n-6:n-3
ratio of the particles is very close tothe one presented
byinnatura oil.Di erential Scanning Calorimetry showed
Figure 8. FTIR spectra of in natura chia oil, chia oil-loaded particles and blank microparticles (no oil added).
(a) DSC under nitrogen atmosphere. (b) DSC under air atmosphere.
Figure 9. DSC thermograms of in natura chia oil, chia oil-loaded particles and blank microparticles (no oil added).
Brazilian Journal of Chemical Engineering
M. F. Souza, C. R. L.Francisco, J. L. Sanchez, A. Guimarães-Inácio,
P. Valderrama, E. Bona, A. A. C. Tanamati, F. V. Leimann and O. H. Gonçalves
an increase in the oxidative stability of the encapsulated oil,
which may indicate that such microparticles are suitable to
formulate food products where long shelf life is needed or
when heating is applied during production such as in baked
Authors thank CAPES, CNPq and Fundação Araucária
for the support.
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... Soy lecithin has been incorporated into the SLM containing vitamin B12 (Cyanocobalamin) [50] and vitamin D3 [37]. Tween 80 and Span 60 were used as surfactants for the encapsulation of curcumin [47] as well as for the formation of Chia oil-loaded microparticles [51]. ...
... Hot homogenization was a suitable technique in view of the natural similarity and compatibility between polyunsaturated fatty acids (PUFA) and the solid lipid carrier. Chia oilloaded solid lipid microparticles were obtained by hot homogenization, using stearic acid as a lipid carrier and Tween 80 as a surfactant at 75 °C [51]. Production of Curcuminloaded solid lipid microparticles was achieved by hot homogenization, as well, using a mixture of tristearin and babacu oil as a lipid carrier and Span 80 as surfactant [47]. ...
... PUFA are susceptible to oxidation that can lead to decreased nutritional and sensory quality. Chia oil was extracted and successfully encapsulated in stearic acid microparticles by hot homogenization method [51]. Researchers found that both omega-3 and omega-6 were effectively encapsulated, maintaining the same omega-3: omega-6 ratio present in natural oil. ...
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Health food has become a prominent force in the market place, influencing many food industries to focus on numerous bioactive compounds to reap benefits from its properties. Use of these compounds in food matrices has several limitations. Most of the food bio-additives are sensitive compounds that may quickly decompose in both food and within the gastrointestinal tract. Since most of these bioactives are highly or partially lipophilic molecules, they possess very low water solubility and insufficient dispersibility, leading to poor bioavailability. Thus, various methods of microencapsulation of large number of food bioactives have been studied. For encapsulation of hydrophobic compounds several lipid carriers and lipid platforms have been studied, including emulsions, microemulsions, micelles, liposomes, and lipid nano- and microparticles. Solid lipid particles (SLP) are a promising delivery system, can both deliver bioactive compounds, reduce their degradation, and permit slow and sustained release. Solid lipid particles have important advantages compared to other polymer carriers in light of their simple production technology, including scale up ability, higher loading capacity, extremely high biocompatibility, and usually low cost. This delivery system provides improved stability, solubility in various matrixes, bioavailability, and targeting properties. This article reviews recent studies on microencapsulation of selected bioactive food ingredients in solid lipid-based carriers from a point of view of production methods, characteristics of obtained particles, loading capability, stability, and release profile.
... According to the Ghena and MB [42], CSO contained 60.69% of ALA (unsaturated fatty acid). In another work, the fatty acid profile showed that the CSO contained 18.11 mg/g ALA [43]. In a similar study carried out by Carrillo et al. [44], the ALA in CSO was 54.08%. ...
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Omega-3 fatty acids are essential fatty acids that our body cannot make itself, so you must get them from functional foods. Therefore, the food processing industries are becoming more inter-ested in production of omega-3 enriched food products, as consumers and healthcare organiza-tions are increasingly demanding functional foods with minimum fatty acid loss and higher ox-idative stability. Moreover, the stability of long chain polyunsaturated fatty acids in functional foods is a major challenge for the food processing industries. Therefore, spray drying method was used to prepared spray dried microcapsules (SDM) with minimum loss and more stable fat-ty acids. Methods: In this study, the emulsion blends of chia seed oil (CSO, 50%) and fish oil (FO, 50%) were spray dried using operating conditions like that, inlet air temperature (IAT) (125, 140, 155, 170, 185°C), wall material (WM) (5, 10, 15, 20, 25%), pump speed (PS) (3, 4, 5, 6, 7mL/min) and needle speed (NS) 3, 5, 7, 9, 11S), respectively. Results: The maximum loss of ALA in spray dried microcapsules (SDM) was estimated (9.90±0.40%) at 170°C and the minimum loss was 4.18±0.20% at run order 9. Similar trend was observed in the maximum retention loss of EPA and DHA (9.71±0.39% and 9.77±0.39%) at high temperature 170°C, while minimum loss of EPA and DHA were observed at run order 9. Furthermore, maximum peroxide value (PV) of SDM was esti-mated at lower temperature 140°C (1.45±0.19meqO2/kg) and minimum PV was 1.33±0.16meqO2/kg. Conclusions: Overall results concluded that the oxidative stability of SDM has been improved and it can be used as a fortifying agent in the processing of many food prod-ucts.
... Souza et al. (47) microencapsulated the chia oil, rich in polyunsaturated fatty acids (omega-3 and omega-6), in order to increase its stability during processing and storage. Differential scanning calorimetry showed an increase in the oxidative stability of the encapsulated oil, which may indicate that such microparticles are suitable to formulate food products where long shelf life is needed or when heating is applied during production such as in baked products. ...
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In addition to being used in food, fuel, and lubricants, vegetable oils are promising in many other applications such as food additives, nutritional supplements, cosmetics, and biomedicine; however, their low oxidative stability can limit their use. Microencapsulation is a well-established methodology for the preservation of oils against degradation, controlled release of active ingredients, protection against external factors during storage, and enhanced durability. In this article, microencapsulation methods for vegetable oils are reviewed, including physical methods (spray drying and freeze-drying), physical-chemical methods (complex coacervation, ionic gelation and electrostatic layer-by-layer deposition), and chemical methods (interfacial/in situ polymerization). This article also provides information on the principles, parameters, advantages, disadvantages, and applications of these methods.
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The present study prepared, optimized, and characterized solid lipid microparticles that contained trans-anethole (SLMAN), evaluated their antiinflammatory activity in acute and chronic inflammation models, and investigated their effects on the gastric mucosa in arthritic rats. The microparticles were obtained by a hot homogenization process and characterized by physicochemical analyses. The acute inflammatory response was induced by an intradermal injection of 0.1 ml of carrageenan solution (200 μg) in the hind paw. The rats were treated orally with a single dose of SLMAN 1 h before induction of the inflammatory response. The chronic inflammatory response was induced by the subcutaneous application of 0.1 ml of complete Freund’s adjuvant suspension (500 µg) in the hind paw. SLMAN was orally administered, starting on the day of arthritis induction, and continued for 21 days. The results showed that SLMAN was obtained with good encapsulation efficiency. Treatment with SLMAN at doses of 25 and 50 mg/kg was as effective as trans-anethole (AN) at a dose of 250 mg/kg on acute and chronic inflammatory responses. Histological analyses showed that treatment with SLMAN did not aggravate lesions in the gastric mucosa in arthritic rats. These results indicated that treatment with SLMAN at a dose that was 5–10 times lower than non-encapsulated AN exerted an inhibitory effect on acute and chronic inflammatory responses, suggesting the better bioavailability and efficacy of microencapsulated AN without aggravating lesions in the gastric mucosa in arthritic rats.
Chia seed oil has a high content of polyunsaturated fatty acids (PUFAs), giving it nutritionally beneficial qualities, although determining its high susceptibility to oxidative deterioration. Microencapsulation and natural antioxidants are alternatives to protect this oil during its processing and storage. This work aims to study the physicochemical characteristics and the oxidative stability of chia seed oil microencapsulated with different antioxidants (rosemary extract, blend of rosemary and chamomile extracts, ascorbyl palmitate) by spray‐drying using sodium caseinate and lactose as wall material. The microencapsulation efficiency and the moisture content were >97% and <3% d.b., respectively. SEM micrographs showed that the microcapsules were spherical, with diameters ranging between 11.3 and 14.8 µm. At t = 0, the microencapsulated oil recorded a ti = 12.7 h, seven times greater than that of the bulk‐oil. The addition of the antioxidants increased the ti of the microencapsulated oil. Regarding the PV, the addition of ascorbyl palmitate maintained the PV under the acceptable limit after 60 d of storage (25°C, darkness, HR 33%). Thus, microencapsulation by spray drying of chia oil with ascorbyl palmitate addition would be the most appropriate studied system to obtain microparticles with high efficiency and oxidative stability during the processing and storage. This article is protected by copyright. All rights reserved This study contributes to investigating the microencapsulation of omega‐3 fatty acids from a novel oilseed (chia oil), applying different antioxidants, including those from vegetable sources such as rosemary and chamomile extracts, to confer additional protection to microencapsulated oil. Thus, the application of these techniques will enable the delivery of this vegetable oil for the development of functional foods.
Microencapsulation of mixture of chia seed oil (CSO) and vitamin D3 (VD3) were studied using the conjugates of soy protein isolate (SPI), maltodextrin (MD) and inulin as wall material by spray drying method. Using response surface, optimized wall material combination was obtained at 5:5:2 for SPI/MD/inulin ratio based on maximum encapsulation efficiency in a constant ratio 1:10 of core /wall of microcapsules. Different core/wall ratios (1:10, 1:8, and 1:5) were prepared using the optimum wall combination. Physicochemical properties of the prepared microcapsules such as encapsulation efficiency, peroxide value, and targeted delivery were determined. The results showed that encapsulation of CSO with SPI/MD/inulin was resulted cover about 88%, encapsulate and entrap the core oil (VD3 and CSO) and protect the oil from oxidation. Also, the microcapsules showed 71‐77% delivery of the core to gastrointestinal tract.
In the present investigation, the emulsion blends of chia seed oil (CSO, 50%) and fish oil (FO, 50%) were spray dried using operating conditions such as inlet air temperature (IAT 125, 140, 155, 170, 185°C), wall material (WM 5, 10, 15, 20, 25%), pump speed (PS 3, 4, 5, 6, 7mL/min) and needle speed (NS 3, 5, 7, 9, 11S), respectively. The highest EE was obtained 83.77±0.96% at 140°C (IAT), 10% (WM), 4mL/min (PS) and 5S (NS) conditions. While, the minimum EE was noted 73.40±0.35% at 170°C (IAT), 20% (WM), 6mL/min (PS) and 9S (NS). The maximum model predicted value of EE was 81.85±0.90%. IAT significantly affected the EE while oxidative quality of spray dried microcapsule (SDM) samples was improved. The sensorial scores of SDM samples were in the acceptable range. Therefore, SDM developed from CSO and FO blends can be recommended for supplementation in different food products.
Omega-3 polyunsaturated fatty acids (PUFA) are important for nutrition and health, by virtue of their importance in lipid homeostasis, and the fact that PUFA deficiencies can increase risk of metabolic syndrome, cardiovascular and neurodegenerative diseases. Chia (Salvia hispanica L.) seeds are rich in PUFA (80%) and contain the highest known levels in plants of the essential omega-3 fatty acid, alpha-linolenic acid (ALA). High degree of unsaturation in edible oils can reduce oxidative stability causing a loss of nutritional value. Nanotechnology can be used to improve chia seed oil quality and safety, increase bioavailability, and expand the scope of applications. Towards this goal, our objective was to prepare and characterize chia seed lipids in the form of nanoliposomes (NL) and nanoemulsions (NE), and to evaluate their potential use as bioactive products. The first step was to characterize lipid fractions. Lipids were extracted from the French ORURO variety of chia seeds using modified Folch method. Ten fatty acid species and six phospholipid (PL) classes were identified in chia seed lipid extract by gas chromatography and LC-MS, respectively, with the highest level of fatty acids being ALA (62%). The presence of a solid residue was detected following evaporation of the solvent to obtain chia seed oil. Analyses by thin layer chromatography and LC-MS demonstrated that this residue contained the polar lipids including PL that were no longer in the chia oil after removal of solvent by evaporation. NE were prepared from chia seed oil and the chia PL-rich solid residue, and NL from the PL-rich solid residue. Physicochemical characterization including analysis of the polydispersity index (PDI), size, and zeta-potential indicated that both NE and NL were monodispersed solutions of stable (low negative zeta potential) particles with a size between 104-118 nm. These preparations were spherical and multilayered (transmission electron microscopy) and remained stable even 5 days after preparation. In addition, enzymatic assay confirmed PL content in both NE and NL. MTT cell viability assay showed little to no cell toxicity (up to 150 µg/mL NE or NL) following 24 h incubation with cultured hepatocytes, neurons, and astrocytes. In conclusion, these results demonstrate the feasibility of using chia lipids for the preparation of stable non-toxic omega-3 PUFA rich NL and NE, which represent potential bioactive vectors for both preventive and therapeutic applications in human health.
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The results of the quantitative determination of fatty acid methyl esters of vegetable oils, (soybean, flaxseed, and palm oils) by eight basic and acid catalysis esterification methods were compared. The selected methods were described by Metcalfe, 1966 (MET, ref. 17); Bannon, 1982 (BAN, ref. 18); Joseph and Ackman, 1992 (JAC, ref. 3); Hartman and Lago, 1973 (HLA, ref. 19); Jham, 1982 (JHA, ref. 20); ISO 5509, 1978 (ISO, ref. 21); Bannon, 1982 (BBA, ref. 15) and Schuchardt and Lopes, 1988 (SLO, ref. 22). Despite the large variation in the determination of unsaturated fatty acids, all the methods were efficient in the analysis of saturated fatty acids. The results obtained show that fatty acid analysis may be affected by oil composition and that JAC, ISO, and BBA methods are more efficient. ISO, and BBA are recommended for low acidity samples due to their low reagent toxicity and cost. The JAC method is recommended only for high acidity samples, as the ISO and BBA methods are carried out in basic medium and cannot analyze the free fatty acids.
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Multivariate Curve Resolution with Alternating Least Squares (MCR-ALS) is a resolution method that has been efficiently applied in many different fields, such as process analysis, environmental data and, more recently, hyperspectral image analysis. When applied to second order data (or to three-way data) arrays, recovery of the underlying basis vectors in both measurement orders (i.e. signal and concentration orders) from the data matrix can be achieved without ambiguities if the trilinear model constraint is considered during the ALS optimization. This work summarizes different protocols of MCR-ALS application, presenting a case study: near-infrared image spectroscopy.
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The oxidative stability of chia oil was evaluated by measuring the effectiveness of the addition of rosemary (ROS) and green tea (GT) extracts, tocopherols (TOC), ascorbyl palmitate (AP) and their blends, and studying the influence of storage conditions. The addition of antioxidants increased induction time, depending on their type and concentration. Considering antioxidants individually, AP at 5,000 ppm was the most effective, whereas ROS + GT at 2,500 and 5,000 ppm provided the best protection among the antioxidant blends. Chia oil peroxide values of 10 mequiv/kg was observed for oils stored at 4 °C while values greater than 10 mequiv/kg were observed between 60 and 120 days when stored at 20 °C. Only AP 2,500 ppm protected oil did not reach 10 mequiv/kg during 225 days at 4 and 20 °C. Similar trends were observed with p-anisidine and Totox values. Differential scanning calorimetry further supported the presence of primary and secondary oxidation. Activation energy of chia oil thermoxidation was 71.9 kJ/mol increasing up to 87.5 kJ/mol when AP was added.
A gas chromatographic (GC) method using a capillary column for analysis of encapsulated fish oils and ethyl esters was studied collaboratively in 21 laboratories. Each collaborator analyzed 6 soft-gelatin encapsulated samples; 5 were trlacylglycerol oils (one was a blind duplicate), and one was an ethyl ester concentrate of omega-3 (n-3) polyunsaturates. Constituent fatty acids of the oils were converted to methyl esters by base-catalyzed transesterlflcatlon of the oils; any free acids in the oils were esterlfied by subsequent reaction with BF3/CH3OH. The ethyl ester concentrate required no further derlvatlzation. Results were reported as area percentages of 24 analytes of nutritional or biochemical interest. In addition, weights (mg/g sample) of EPA (all-c/s-5,8,11,14,17-elcosapentaenolc acid or 20:5n-3) and DHA (all-c/s- 4,7,10,13,16,19-docosahexaenoic acid or 22:6n-3) were determined through the use of the internal standards, respectively, methyl tricosanoate (23:0) and ethyl 23:0, for the methyl and ethyl esters. The only instrumentation specifically required was a flexible fused silica capillary GC column coated with a bonded polyglycol such as Carbowax-20M, an oxygen scrubber Installed In the carrier gas supply line, and a flame Ionization detector (FID). Most of the collaborators experienced little difficulty In applying the method, and, of 2526 values reported, only 4.3% were identified as outlier values. The reproducibility relative standard deviations (RSDR) compared favorably in most instances with, or were substantially better than, those of 2 earlier collaborative studies of fish oils. Because the variances were homogeneous, standard deviations and relative standard deviations determined on the area percent analyses of the blind duplicate oils were pooled to give the following mean values: sr = 0.15, RSDr = 4.88%, sR = 0.41, and RSDR = 12.91%. Analytes that rarely occur at greater than 0.5% In marine oils (22:0,22:4n-6,22:5n-6,24:0, and 24:1) were not Included in these calculations. The method was adopted first action by AOAC International as an American Oil Chemists' Society (AOCS)-AOAC method.
BACKGROUND The lipids of 16 farmed and wild European sea bass (Dicentrarchus labrax) samples were studied by Fourier transform infrared (FTIR) spectroscopy. The spectroscopic parameters which would be useful when distinguishing between both fish origins were analysed.RESULTSIt was shown, for the first time, that the frequency and the ratio between the absorbance of certain bands are efficient and reliable authentication tools for the origin of sea bass. Furthermore, relationships between infrared data and fish lipids composition referring to the molar percentage or concentration of certain acyl groups were also studied. It was proved that some infrared spectroscopic data (the frequency of certain bands or the ratio of the absorbance of others), are very closely related to the composition of sea bass lipids. It was shown for the first time that certain infrared spectroscopic data could predict, with a certain degree of approximation, the molar percentage, or concentration, of omega-3, docosahexaenoic (DHA) and di-unsaturated omega-6 (linoleic) in sea bass lipids.CONCLUSION The consistency of the results confirms the usefulness of FTIR spectroscopy to detect frauds regarding sea bass origin, and to provide important compositional data about sea bass lipids from the nutritional and technological point of view. © 2013 Society of Chemical Industry
The processing parameters related with chia oil extraction employing screw press have not been studied yet. A Box–Behnken experimental design was used to study the optimization process by response surface analysis. The independent variables considered were seed moisture content, restriction die, screw press speed and barrel temperature, while the response variables measured were oil yield, fines content in oil and oil quality (acidity, peroxide index, K232, K270, values, antioxidant activity and total tocopherol content). Since chemical quality data of chia seeds oil pressed at different conditions was not affected, the response was optimize to maximize oil yield. The results suggested that 0.113 g/g dry solids (0.101 g/g seed), 6 mm restriction die, 20 rpm screw press speed and 30 °C barrel temperature were the best processing combination to maximize oil yield.
a b s t r a c t Eight chia essential oil-in-water fresh emulsions (E) variations were prepared using biopolymers blends whey protein concentrate (WPC) with mesquite gum (MG) or gum Arabic (GA), core to wall material ratios (C o :W a) of 1:2 and 1:3, and total solids contents (TSC) of 30 and 40 wt%. All E variations displayed volume-weighted mean size (d 4,3) droplet sizes that fell within 2.32 and 3.35 lm and rates of droplet coalescence (k C) of 10 À8 s À1 . E variations were spray-dried and the resulting microcapsules (M) had d 4,3 falling within the range of 13.17–28.20 lm. The encapsulation efficiency (EE) was higher than 70% for all M, but those obtained from E with lower TSC and higher C o :W a displayed higher EE and lower surface oil, independently of M particle size. The reconstituted emulsions (RE) exhibited significantly higher d 4,3 and k C values of the same magnitude as E variations.