Journal of Food Engineering 112 (2012) 2937

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Journal of Food Engineering

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Preparation and characterization of non-aqueous extracts from chilli (Capsicum

annuum L.) and their microencapsulates obtained by spray-drying
Andrea Yazmin Guadarrama-Lezama a, Lidia Dorantes-Alvarez a, Maria Eugenia Jaramillo-Flores a,
Csar Prez-Alonso b, Keshavan Niranjan c, Gustavo Fidel Gutirrez-Lpez a, Liliana Alamilla-Beltrn a,
a
Departamento de Graduados e Investigacin en Alimentos, Escuela Nacional de Ciencias Biolgicas, Instituto Politcnico Nacional, Carpio y Plan de Ayala s/n, CP 11340 Mxico,
DF, Mexico
b
Facultad de Qumica, Universidad Autnoma del Estado de Mxico, Paseo Tollocan esq. Paseo Coln s/n, CP 50120 Toluca, Estado de Mxico, Mexico
c
Department of Food and Nutritional Sciences, University of Reading, Whiteknights, P.O. Box 226, Reading G66AP, UK

a r t i c l e

i n f o

Article history:
Received 16 November 2011
Received in revised form 1 March 2012
Accepted 10 March 2012
Available online 30 March 2012
Keywords:
Chilli
Carotenoids
Non-aqueous extract
Antioxidant activity
Microencapsulates

a b s t r a c t
Antimicrobial, antioxidant, and pro-vitamin properties have been attributed to Capsicum based on the
carotenoid and polyphenolic compound content. The aim of this study was to obtain and characterize
non-aqueous extracts of Capsicum annuum L. (chilli) using three different oils (corn, sunower, and safower) as well as their microencapsulates. Corn extract showed better antioxidant activity and total
carotenoid content (as b-carotene) than sunower and safower extracts. The extracts were encapsulated
by spray-drying with a biopolymers:extract-solution ratio of 4:1 (w/w). The biopolymers were gum
Arabic and maltodextrin. In addition, the encapsulation efciency, mean particle size, morphology, water
activity, moisture content, and stability were evaluated for the microcapsules. The retention of antioxidant activity after encapsulation varied from 76% to 80% of its activity in the oily extract, whereas the
preservation of carotenoids in microcapsules was between 84% and 86%.
2012 Elsevier Ltd. All rights reserved.

1. Introduction
Capsicum annuum L. (chilli) is widely used for culinary and
industrial purposes due to its characteristic avour and colour
(Topuz et al., 2009). Antimicrobial, antioxidant/free-radical, and
pro-vitamin properties have been attributed to C. annuum, given
its content of polyphenolic compounds and carotenoids
(Acero-Ortega et al., 2005; Hornero-Mendez et al., 2000; Topuz
and Ozdemir, 2007). Chillies are good sources of carotenoids;
approximately 25 different carotenoids have been identied in
C. annuum L. grossum Sendt, including b-carotene, a-carotene,
b-cryptoxanthin, zeaxanthin, luteine, capsanthin, capsorubin,
and cryptocapsin, which are the most abundant components
(Collera-Ziga et al., 2005). Provitamin A, carotenoids (bcarotene, a-carotene, and b-cryptoxanthin), and xanthophylls
may be important for the prevention of age-related macular degeneration and cataracts (Matsufuji et al., 1998; Seddon et al., 1994).
The antioxidant activity of the carotenoid pigments is due to the
following characteristics of their structure: (a) the polyene carbon
chain, which permits the incorporation of free radicals by addition
mechanisms, which slows propagation, and (b) functional groups
on the b-rings, such as keto groups as well as the esteried form,
Corresponding author. Tel.: +52 5557296000x62464.
E-mail address: liliana.alamilla@gmail.com (L. Alamilla-Beltrn).
0260-8774/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.jfoodeng.2012.03.032

which potentiate the antioxidant activity (Prez-Glvez and

Mnguez-Mosquera, 2002). Therefore, the use of chilli peppers as
ingredients could be a useful alternative for designing functional
foods that contain high antioxidant activity. More recently, there
has been interest in extracting bioactive compounds, such as
carotenoids from vegetables and fruits, because of the potential
of these substances as functional ingredients in food formulations
and nutritional supplements (Marete et al., 2009). Because of their
hydrophobic nature, carotenoids are generally extracted from
plant materials using organic solvents (Craft, 1992). The carotenoids in Capsicum are commonly extracted with hexane because
of the low-polarity nature of these compounds. Recently, Richins
et al. (2010) compared two methods for carotenoids extraction
from Capsicum: the rst by using hexane, and the second by means
of supercritical uid extraction (SFE) with CO2. The efciency of
extraction by SFE was 31% greater than that obtained with hexane.
In order to improve this result, ethanol was used in addition to SFE
for recovering the carotenoids. Although new methods for extraction of bioactive compounds have been developed, the use of
solvents, which cannot be consumed, has not been totally eradicated. Solvents used for carotenoid extraction must be removed
from the extracts before they can be included in foods, which requires an additional step in the process. Therefore, new methods
for extraction and preservation of the antioxidant properties of
carotenoids are needed. In this context, the use of edible oils as

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A.Y. Guadarrama-Lezama et al. / Journal of Food Engineering 112 (2012) 2937

extraction media may be a novel option for non-aqueous extraction processes that have potential advantages in health, safety,
and ecologically-related issues. To date, the use of edible oils as
non-polar dissolvents for the extraction of carotenoids from Capsicum has not been explored. Once carotenoids are extracted, isomerization (Xianquan et al., 2005) and oxidative reactions may occur
as a consequence of the exposure of carotenoids to ambient temperature and oxygen as well as the presence of unsaturated double
bonds in the molecular structure of carotenoids, which causes molecule fractioning and the production of apocarotenoids (Maoka
et al., 2001) or epoxides. For this reason, the extracts must be
carefully handled. However, one possible approach for minimizing
or inhibiting deteriorative reactions of carotenoids in extracts of
Capsicum is by protecting the extracts in microcapsules.
Microencapsulation through spray-drying is an effective technique that allows for the protection of food ingredients, such as
carotenoids (Rocha et al., 2012) and polyphenols (Fang and Bhandari, 2010), from chemical deterioration and environmental factors
by converting liquids into functional powders that can be incorporated into various formulations. This protection was performed
using wall materials, such as sugars, gums, proteins, natural and
modied polysaccharides, lipids, and synthetic polymers (Gharsallaoui et al., 2007; Fang and Bhandari, 2010; Rocha et al., 2012).
It has been reported that both protein and lipid fractions that are
part of the molecular structure of gum Arabic provide emulsifying
properties, lm formation, low viscosity and high water solubility
(Yadav et al., 2007). Similarly, it has been postulated that more
hydrophobic polypeptide chains adsorbed at the surface of the oil
droplets with hydrophilic carbohydrate blocks attached to the
chain protruding out into solution can provide a stronger steric
barrier that prevents droplet aggregation and coalescence (Islam
et al., 1997). Maltodextrin exhibits various favourable characteristics, including high hydrosolubility, low emulsifying capacity, low
retention of volatiles, and high protection against oxidation (Buffo
and Reineccius, 2000). During microencapsulation by spray-drying,
dry particles are obtained in the form of powders or agglomerates
that can enhance the shelf-life of food products (Soottitantawat
et al., 2005). Based on these studies, the objective of this work
was to explore the extraction of carotenoids from chilli peppers
by using non-aqueous media, such as edible oils, and the preservation of the extracted compounds in the form of microcapsules,
which could be used as an ingredient in food processing.
2. Materials and methods
2.1. Materials
The C. annuum L. grossum Sendt (chilli) used for this work as
well as the corn (Maceite), sunower (Patrona) and safower
(Oleico) oils were purchased from a local market in Mexico City,
Mexico. The wall materials used for microencapsulation were
gum Arabic, food grade E 414 (Distribuidora Qumica LEFE S.A de
C.V., Mexico City, Mexico) and maltodextrin 20 DE (CPI Ingredientes S.A de C.V, State of Mexico, Mexico). Potassium persulfate
(K2S2O8) and 2,2-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid
(ABTS) radical were purchased from Sigma Chemical Company,
St. Louis, MO, USA.
2.2. Methods
2.2.1. Extraction of carotenoids from C. annuum L. grossum Sendt
(chilli)
Dried chilli peppers were selected and manually cleaned to
eliminate foreign matter. The stems were also removed prior to
dry grinding. The resulting powder was sieved using a 25 mesh

(Tyler Standard Sieve Series, Mentor, Ohio, USA). Extraction was

performed using corn, sunower, and safower oils at three different temperatures (60, 70, and 80 C) and two mixing times (5 and
10 min). In all cases, the chilli powder and oil was mixed at a 1:2
(w/v) ratio, respectively, at 1100 rpm in a Thermomix (TM 31, Vorwerk, Spain). Rened and comestible oils were used for extraction.
Corn, sunower, and safower oils have 12%, 10%, and 7.4%
saturated fatty acids, respectively; palmitic and stearic acids are
present in the highest concentration in the four oils. In addition,
these oils contain 88%, 90%, and 92.6% unsaturated fatty acids,
respectively, with oleic and linoleic being the most abundant.
The obtained extracts were ltered through cheesecloth and subsequently centrifuged (Allegra X-12R Beckman Coulter, USA) at
3700 rpm for 15 min to separate the solids and to obtain the
non-aqueous extracts of chilli (NAEC). The NAEC were stored in
amber glass recipients at 10 C for further use.
2.2.2. Determination of antioxidant activity of NAEC using the
2,20 -azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS)+
method
The antioxidant activity of the extracts was determined by
diluting 200 lL NAEC with 800 lL of acetone (Fermont, Mxico).
Of this solution, 10 lL was reacted with 990 lL of ABTS+ radical,
and the absorbance was measured at 734 nm (Pastrana-Bonilla
et al., 2003). All measurements were performed in triplicate, and
the average standard deviation (SD) was reported. The percent
inhibition was calculated as follows:

Ast0  Astf
h
i
%Inhibition 
Adt0 Adtf
Ast0 
Adt 0

where Ast0 and Astf are the absorbance of sample at initial and nal
times; Adt0 and Adtf are the absorbance of dissolvent at initial and
nal times.
A standard curve was constructed using different concentrations of Trolox (6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid; Sigma Chemical Company, St. Louis, MO, USA). The
results were presented as lmol Trolox/mL. The antioxidant activity
determined for pure oils were subtracted from the antioxidant
activity of the extracts.
2.2.3. The Folin test
The Folin test for NAEC and NAEC microcapsules was determined
using the FolinCiocalteau reagent (Sun et al., 2007). The reagent
was diluted 10 times with deionized water. Each NAEC was diluted
at a ratio of 1:5 with ethanol, and a 0.1 mL aliquot was mixed with
0.75 mL of the diluted FolinCiocalteau reagent. After the reaction
solution had been incubated at room temperature (RT) for 5 min,
0.75 mL (60 g/L) sodium bicarbonate solution was added and thoroughly mixed. The mixture was incubated at RT for 90 min and then
ltered by using a 0.45 lm syringe lter (Corning, Germany). The
absorbance of the solution was then determined at 750 nm. Gallic
acid was used as standard reference and the results were expressed
as gallic acid equivalents (lg) per mL of extract.
2.2.4. Extraction of carotenoids with fatty acids
Carotenoid extracts of chilli powder were obtained through
homogenization with stearic and oleic acids at 70 C for 5 min to
evaluate carotenoid afnity with saturated or unsaturated fatty
acids. This temperature of extraction was selected due to the fact
that stearic acid is in a solid state below 70 C.
2.2.5. Preparation of oil-in-water (o/w) emulsions and the spraydrying process
Gum Arabic (GA; 10 g) and maltodextrin (MD; 10 g) were
dissolved in 100 mL of distilled water using a mixer (Stir-Pak

A.Y. Guadarrama-Lezama et al. / Journal of Food Engineering 112 (2012) 2937

Laboratory Stirrer, Cole Palmer Instrument Co., Model 4554-00,

USA). This solution was stored at 10 C overnight to ensure complete rehydration of the polymers (Prez-Alonso et al., 2008). Three
oil-in-water (o/w) emulsions were prepared by adding each of the
three different non-aqueous extracts prepared with corn, sunower, and safower oil drop-by-drop to the biopolymeric solution, while homogenizing the solution with an Ultra-Turrax
(M45, USA) at 10,000 rpm, with U = 0.05 (relation of the volume
of the dispersed phase to the total volume of the emulsion) and a
biopolymers:extract ratio of 4:1. Once the oil was added, homogenization was continued for an additional 3 min. An ice bath was
used during the preparation of the emulsions with the goal of
maintaining temperature under 30 C in order to avoid instability
of the system (Koberstein-Hadja and Dickinson, 1996). The emulsion was fed into the spray-dryer (Mobile Minor 2000, GEA Niro,
Denmark) using a peristaltic pump (Watson-Marlow 520S, USA).
The spraying system was a pneumatic nozzle with parallel
arrangement in respect to the air ow. The inlet and outlet temperatures of drying air used for the microencapsulation were
160 2 C and 70 2 C, respectively, and an air pressure of
0.4 kg/cm2 was used for spraying. The liquid feed rate was
13.3 mL/min. The microencapsulated NAEC were collected and
placed into plastic bags, hermetically sealed, and stored at
25 2 C in the absence of light until further characterization analyses were performed.

2.2.6. Evaluation of antioxidant activity and Folin test of

microencapsulated NAEC
Two grams of microcapsules were dissolved in 3 mL of bidistilled water at 50 C by stirring for 3 min in a Vortex (Maxi Mix
II, Barnstead Thermolyne, USA) followed by the addition of
10 mL of hexaneisopropanol (3:1) (Hardas et al., 2000). The mixture was vortexed for an additional 5 min and centrifuged at
3600 rpm for 15 min at 10 C. The mixture NAEC-solvent phase
was separated using a Pasteur pipette and placed into a 50 mL
round-bottom ask. The solvent was evaporated to a nal volume
of 2 mL at 50 C using a rotary vacuum evaporator (Buchi R-210/
R-215, Flawil, Switzerland). Antioxidant activity and the Folin test
were determined by using the ABTS+ free radical scavenging
method described in Section 2.2.2 and the Folin test described
in Section 2.2.3.

2.2.7. Determination of total carotenoid content in NAEC and

microencapsulated NAEC
The carotenoid content (CT) as well as red (CR) and yellow
(CY) isochromatic fractions were spectrophotometrically determined using the method proposed by Hornero-Mndez and
Mnguez-Mosquera (2001). This method consists of reading the
absorbance of the carotenoid solutions, which were obtained by
mixing 0.4 mL of NAEC with 2 mL of acetone, at 472 and 508 nm.
In the case of microencapsulated NAEC, the rst step was to
separate the oil fraction (containing carotenoids) from the biopolymers (GA and MD) as described in Section 2.2.6. Removal of the
hexane:isopropanol was performed by gasing out using nitrogen.
The oil fraction was nally diluted with acetone and its absorbance
at 472 and 508 nm was evaluated. In this work, total carotenoid
content is expressed as b-carotene content.

2.2.8. Evaluation of water activity and moisture content of

microencapsulated NAEC
The water activity of the microcapsules was determined using
an Aqualab (Decagon Devices, Model 4 TE, USA) at 25 C. Moisture
content of the microcapsules was determined gravimetrically
using the ofcial AOAC method (AOAC, 1995).

31

2.2.9. Morphology of microcapsules by scanning electron microscopy

(SEM)
The morphology and appearance of the surface of microcapsules of NAEC obtained by spray-drying were examined with a
scanning electron microscope (SEM; Jeol, Model JSM-5800LV,
Japan). Samples of microcapsules of NAEC were sprayed with a
paintbrush to a metal die, which had a two-sided adhesive carbon
tape attached to it (Ted Pella, Redding, California, USA). The samples were subsequently coated with gold ions (Rosenberg and
Young, 1993) using a magnetron sputter coater (Denton Vacuum,
Model Desk II, USA) at 13.3 kPa and 15 mA. The coated samples
were then observed using SEM, which was operated at an accelerating voltage of 15 kV (Jafari et al., 2007), and the corresponding
images were captured.
2.2.10. Determination of extractable and non-extractable NAEC in
microcapsules
In order to determine the non-extractable fraction of NAEC,
which was the percent of encapsulated NAEC, 2 g of microcapsules
were added to 20 mL of hexane. Agitation was performed for 5 min
to avoid transfer of the NAEC from the internal part to the outer
part of the microcapsules. Once agitation concluded, the powder
and the solvent were separated by ltration through grade 1 Whatman lter paper and the residual solid was washed out with 5 mL
of solvent. The ltered solution was transferred to a round-bottom
ask for complete evaporation of the solvent using the rotary vacuum evaporator (Buchi R-210/R-215, Flawil, Switzerland). The
residual solids were dissolved following the procedure described
in Section 2.2.6, which included complete evaporation of the solvent to determine the amount of encapsulated NAEC or nonextractable fraction (Drusch and Berg, 2008; Calvo et al., 2010).
The percent of encapsulated NAEC was calculated using:

Eo

AT  AS
AT

x100

where AT and AS are the total content of NAEC and the content of
extractable portion of encapsulated NAEC, respectively.
2.2.11. Encapsulation efciency (EE)
The EE was calculated as the ratio between the initial content of
total carotenoid present in the capsules and the total carotenoid
content in the extract used to produce them. The EE was analysed
based on b-carotene as a target chemical compound that has been
reported as the major component in chilli (Collera-Ziga et al.,
2005). The total carotenoid content in extracts and microcapsules
(as b-carotene content) was determined using the procedure described in Section 2.2.7.
2.2.12. Determination of the mean particle size of microcapsules
A particle size analyzer (Mastersizer 2000, Malvern Instruments
Ltd., Malvern, Worcestershire, UK) was used to determine the
Sauter mean diameter (d3,2) of the particles (Jafari et al., 2007).
2.2.13. Stability tests for microencapsulates
The stability of microencapsulated NAEC was determined by
measuring the antioxidant activity (Section 2.2.6) and water activity (Section 2.2.8) of the microcapsules after 60 d of storage at
20 5 C.
2.2.14. Statistical analysis
A one-way analysis of variance (ANOVA) with 2a = 0.05 signicance level was applied to all results. The Tukeys test was used to
compare differences between mean values of individual samples
(Minitab 15.0 software, Minitab Inc., USA).

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A.Y. Guadarrama-Lezama et al. / Journal of Food Engineering 112 (2012) 2937

3. Results and discussion

3.1. Extraction conditions, antioxidant activity, and Folin test
Data of antioxidant activities from all extraction conditions are
shown in Table 1. The best extraction of carotenoids and optimal
antioxidant activity in the extracts was obtained when extraction
was conducted at 60 C for 5 min while mixing at 1100 rpm. The
highest temperatures (70 and 80 C) and longer extraction times
had a negative effect on the antioxidant activity of NAEC. The type
of oil used for the extractions inuenced the antioxidant activity
and exhibited different afnities for the carotenoids (Table 2).
The extract obtained with corn oil at 60 C and 5 min had signicantly (p 6 0.05) higher antioxidant activity (78.5 0.7 lmol-Trolox/mL) than the sunower and safower oil extracts (67.3 1.1
and 51.7 0.1 lmol-Trolox/mL, respectively). Similar results were
observed for the yellow and red fractions and total carotenoid content for oily extracts of corn, sunower, and safower, respectively
(Table 2). The antioxidant activities found for pure oils were
20.9 0.8, 17.8 0.5, and 13.1 0.6 lmol-Trolox/mL for corn, sunower and safower oils, respectively, and were subtracted from
the antioxidant activity values reported for the extracts.
Carotenoids are non-polar compounds that are soluble in nonpolar solvents, oils, and fats. These are present in plants in free
form or esteried (most of them). The hydrophobicity, stability,
and antioxidant activity of the carotenoids depend on the type of
fatty acid to which the carotenoid is esteried (Ramakrishnan
and Francis, 1979; Schweiggert et al., 2007; HongFei et al., 2010).
However, capsanthin as well as its various esters inhibit the oxidation process in a similar manner to unesteried capsanthin, suggesting that the radical scavenging ability is not inuenced by
esterication (Matsufuji et al., 1998). The composition, degree of
unsaturation, and the length of the fatty acid chains of different oils
have a strong inuence on their afnity by carotenoids, and therefore the extracts obtained with each type of oil have a different
composition of carotenoids and consequently a different antioxidant activity. Corn oil, which contains a higher proportion of saturated fatty acids (12%) compared to sunower and safower oils
(10% and 7.4%, respectively), is a better media for extracting carotenoids with antioxidant activity.
The antioxidant activity of chilli extracts prepared using stearic
acid (18C-saturated acid) as extractive media was 90.2 2.5 lmolTrolox/mL, whereas extracts prepared with oleic acid (18C-unsaturated acid) had an antioxidant activity of 63.1 3.5 lmol-Trolox/

mL. These results suggested that saturated fatty acids had a better
afnity for carotenoids and exhibited enhanced stability compared
to extracts obtained by using unsaturated fatty acids, despite both
types having hydrocarbon chains of 18 carbon atoms. Carotenoids
consist of a skeleton of 40 unsaturated carbon atoms, which provides
hydrophobic specicity, and differences in the antioxidant activity of
extracts may be due to a higher chemical afnity of carotenoids for
saturated fatty acids than for unsaturated fatty acids in the oils. This
may be due to differences in the molecular conformation of
saturated and unsaturated fatty acids, which have one or more rigid
torsions in their hydrocarbon chains due to the inability to present
bond rotation. In the case of saturated fatty acids, the extended form
(linear) conguration prevails because this structure has the lowest
energy (Lehninger et al., 1995; Kaneko et al., 1998).
Hyeon and Young (2008) evaluated the antioxidant activity of
seed and pericarp of red pepper. Extraction was performed with
70% ethanol for 3 h, and antioxidant activity was measured using
various chemical assays, including the ABTS+ method. The seed
showed a radical scavenging activity of 29% at 1000 lg/mL extract,
while pericarp had 51% activity. In our study, the NAEC of corn,
sunower, and safower oils showed 90%, 75%, and 60% radical
scavenging by ABTS+, respectively. The values observed by Hyeon
and Young (2008) were lower than those obtained with NAEC,
which may be due to the different mechanisms of action that phenolic compounds, avonoids, and carotenoids have in the presence
of the ABTS radical. The NAEC were obtained at moderate temperature and extraction time (60 C and 5 min), which further reduced
the possibility of compound degradation and represents a technological advantage for food-related applications, since volatile solvents were not used for the extraction.
Table 1 shows the results of the Folin test and antioxidant activity, which demonstrated that the highest temperature used for
extraction (80 C) and longer time to homogenization (10 min)
caused a negative effect on the compounds detected. The highest
antioxidant activity was observed in extracts made with corn oil.
Therefore, the compounds detected by the Folin reagent play an
important role in the antioxidant activity of non-aqueous extracts
of chilli.
3.2. Antioxidant activity, carotenoid content, and Folin test of
microencapsulated NAEC
All microencapsulated NAEC collected from the drier retained
7680% of the antioxidant activity of the respective extracts (Table

Table 1
Conditions of extraction, antioxidant activity, and Folin test of NAEC.
Oils used for extraction

Temperature (C)

Time (min)

Antioxidant Activity of
NAEC (lmol Trolox/mL)

Folin test of NAEC expressed

as (lg gallic acid/mL)

Corn

60
60
70
70
80
80

5
10
5
10
5
10

78.5 0.7a
83.1 2.0a
68.2 1.6b
55.9 0.5c
61.3 2.3d
52.2 2.4e

57.3 0.7a
63.5 0.6b
40.6 0.4c
55.8 1.4a
45.7 0.4d
47.4 1.8d

Sunower

60
60
70
70
80
80

5
10
5
10
5
10

67.3 1.1a
60.9 0.4b
43.7 2.5c
46.3 1.8c
51.4 2.0d
38.4 0.2e

50.3 0.4a
57.9 0.8b
36.4 1.4c
40.2 1.9c
35.6 0.3c
26.6 0.5d

Safower

60
60
70
70
80
80

5
10
5
10
5
10

51.7 0.1a
36.9 0.9b
47.1 1.0c
35.4 0.4b
48.3 0.3c
42.1 0.6d

32.3 0.1a
27.9 0.4b
30.8 0.7a
37.2 0.3c
32.8 0.2a
18.3 0.4d

Statistical analysis was performed by the type of oil used, and different letters in the same column indicate signicant difference at p 6 0.05.

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A.Y. Guadarrama-Lezama et al. / Journal of Food Engineering 112 (2012) 2937

Table 2
Red fraction, yellow fraction, and total carotenoid content as determined by bcarotene (lg/mL) content of NAEC by oil type.

Red fraction (CR)a

Yellow fraction (CY)a
Total carotenoid content as bcarotene (lg/mL)

Corn

Sunower

Safower

72.0 0.5a
159.1 1.8c
231.1 2.3e

68.4 0.6b
153.1 0.4c
221.4 1.1f

64.4 1.0b
144.3 0.5d
208.6 6.0f

Statistical analysis was performed by the type of oil used for extraction, and different letters indicate signicant difference at p 6 0.05.
a
Isochromatic families are CR: capsanthin and capsorubin; CY: zeaxanthin, bcryptoxanthin, and b-carotene.

3). A similar retention of antioxidant activity (82%) was reported

for encapsulated beetroot juice processed by spray-drying (Pitalua
et al., 2010) when GA was used as an encapsulant agent.
The carotenoid content of the microencapsulated NAEC is
shown in Table 3; approximately 80% of the total carotenoid content was preserved, which suggests that this process is a good
method for conserving carotenoid content. In microencapsulated
NAEC of corn, sunower, and safower oils, the content of phenolic
compounds and compounds detected with Folin reagent represented only 7.01%, 6.57%, and 4.64% of the total, respectively. These
results suggest that phenolics compounds and other compounds
detected by Folin reagent are more susceptible to degradation during the microencapsulation process.

3.3. Water activity and moisture content of microencapsulated NAEC

The water activity and moisture content of the microcapsules is
presented in Table 3. The average water activity of the microcapsules was between 0.15 and 0.19, and the moisture content was
3.955.10% (dry base). No signicant difference was found in water
activity (p P 0.05). Among the parameters that determine the stability of encapsulated bioactive compounds are moisture content
and water activity; therefore, it is important to understand and
have good control of these parameters during the processing and
storage of powders. Reineccius (2004) reported that when moisture content reaches values lower than 7%, water diffusion through
the food matrix decreases, which reduces the effect of moisture
content on the physical and chemical characteristics of the solid
matrix of microencapsulated oils and the accessibility of oxygen
to oil through the porous network. On the other hand, low values
of water activity (p 6 0.5) have been associated with decreased
degradation of components of the food powder. In our study, the
water that was available to carry out reactions of degradation by
chemical-enzymatic mechanisms was low, and consequently the
degradation of the components of the microencapsulated NAEC
was also low.

3.4. Morphology of microcapsules by SEM and mean particle size

Samples were examined by SEM order to determine the presence of fractures, cracks, or any other possible defects that could
expose unencapsulated NAEC, since any fracture may lead to the
degradation and oxidation of the exposed encapsulated material.
In all cases, the SEM images showed the presence of semi-spherical
microcapsules, which showed dents and rough surfaces, but no
evidence of fracture (Fig. 1).
The existence of different morphologies and surface irregularities is a function of the composition of the feed, droplet size, and
temperature during the drying process (Handscomb and Kraft,
2010). In some cases, shrinkage of the particle followed by an
incipient expansion may induce changes in the size of particles
and broken shells (Alamilla-Beltrn et al., 2005). The typical shape
of spray-dried particles is spherical, with a mean size of
10100 mm (Fang and Bhandari, 2010). In the NAEC microcapsules, no fractures were observed, which may be due to the low
drying temperature as well as viscoelastic and lm-forming
properties provided by the GA (Jimnez-Avalos et al., 2005;
Gharsallaoui et al., 2007) that allow for better physical protection
and retention of carotenoids (Table 3). In addition, the irregularity
on the surface of the microcapsules may be desirable in terms
of enhanced dispersibility and rehydration of the powders
(Prez-Alonso et al., 2009).
The Sauter (d3,2) diameter for the different types of microcapsules is shown in Table 3. The highest value of d3,2 was observed
for the microcapsules obtained with safower oil (approximately
12 lm). Jafari et al., 2007 studied emulsions of d-limonene and sh
oil with Hi-Cap and WPC as wall materials and reported that particle size could be related to the amount of extractable oil. They
also found that it is possible to have more extractable oil on the
surface of large particles than on small particles; however, in the
NAEC microcapsules, no signicant differences (p 6 0.05) were
found in particle size of the fraction of non-encapsulated oil. Therefore, the mean particle size is an important factor in terms of quality and the possible application of the microcapsules. The span
values for the microcapsules of NAEC were 2.47 0.2, 2.21 0.3,
and 1.73 0.2 using corn, sunower, and safower oils for extraction, respectively. In all cases, the low span values indicated a
monodisperse distribution of mean size particle (Jimnez-Alvarado
et al., 2009).
Although microcapsules made with safower oil extract had a
tendency towards monodispersity (Fig. 2), they had the highest
mean particle size, which may be due to the fact that this oil modied the characteristics of the surface of particles undergoing drying as well as size and viscosity of the emulsion. Tcholakova et al.
(2011) found that the Sauter diameter (d3,2) increased in emulsions
as the viscosity of the oily phase increased (hexadecane, mineral
oils, and silicone oils, which had different values of viscosity).

Table 3
Characteristics of microencapsulated NAEC obtained from three different extracts.

Antioxidant activity (%)a

Red fraction (CR)b
Yellow fraction (CY)b
Total carotenoid content as b-carotene (lg/mL)
Moisture content (%)
Water activity (aw)
Encapsulated NAEC (%)
Encapsulation efciency (%)
Sauter diameter (d3,2) (lm)

Corn

Sunower

Safower

80.5 3.1a
60.3 0.5c
139.9 0.04e
200.3 0.6g
4.0 0.05j
0.15 0.01l
90.7 0.5m
86.6 1.4n
11.8 1.5o

80.0 3.1a
58.8 0.6c
126.9 1.1f
185.8 0.5h
5.0 0.1k
0.18 0.01l
90.4 0.6m
83.9 1.5n
11.1 1.4o

76.5 3.1b
53.3 0.2d
122.4 0.9f
175.8 0.7i
3.9 0.03j
0.19 0.01l
91.6 0.6m
84.2 1.0n
12.7 0.5o

Statistical analysis was performed by the type of oil used for extraction, and different letters indicate a signicant difference at p 6 0.05.
a
Values based on the antioxidant activity with respect to the non-aqueous extracts.
b
Isochromatic families are CR: capsanthin and capsorubin; CY: zeaxanthin, b-cryptoxanthin, and b-carotene expressed as lg/mL of extract.

34

A.Y. Guadarrama-Lezama et al. / Journal of Food Engineering 112 (2012) 2937

Fig. 1. Scanning electron microscopy (SEM) micrographs of the microcapsules obtained from extracts using (a) corn oil, (b) sunower oil, and (c) safower oil.

The viscosity of the rened oils, which constitute the oil phase of
emulsions, was found to be 51.44 (25 C), 48.98 (25 C), and 52
(30 C) cP for corn, sunower, and safower oils, respectively
(Abromovic and Klofutar, 1998; Khtoon and Krishna, 1998; Rogers
et al., 2011).

3.5. Encapsulated NAEC and encapsulation efciency

Two wall materials were chosen based on a consideration of
important characteristics, such as solubility and the capacity to
protect against oxidation. In order to select the wall material for
microencapsulation, the optimal mixture of GA and MD was rstly
determined, and different ratios of core:wall material were tested.
It has been reported that when the concentration of oil in an emulsion preparation is 5%, better homogenization and high encapsulated oil were are obtained (Martins and Kieckbusch, 2009).
Emulsions and microcapsules were prepared in 1:1, 2:1, and 1:2
(GAMD) ratios at a nal concentration of 20% solids and 5% oily
phase. The results showed that a ratio of 1:2 (GAMD) preserved
90% of the antioxidant activity of the extract, while a ratio of
2:1(GAMD) only preserved approximately 77% of the activity.
However, the uncapsulated NAEC at a ratio of 1:2 was 49.3% and
ratio of 2:1 was 17%, which is unfavorable in terms of NAEC
conservation, since greater exposure increases the susceptibility

Fig. 2. Distribution of particle size for the microcapsules obtained from extracts
using corn oil, sunower oil, and safower oil.

A.Y. Guadarrama-Lezama et al. / Journal of Food Engineering 112 (2012) 2937

to degradation. At a ratio of 1:1 (GAMD), 80% of the antioxidant

activity was preserved, while approximately 86% of the extract
was encapsulated and therefore less prone to degradation by environmental factors. Therefore, this ratio of wall materials was used
to encapsulate the extracts. Spray-drying is generally performed at
180220 C, and 6080 C is used for inlet and outlet air temperatures, respectively (Sabliov and Astete, 2008; Tonon et al., 2011).
Based on this range of temperatures, we performed the microencapsulation of NAEC at two different temperatures. Using inlet/
outlet drying air temperatures of 170/90 C, respectively, the powder recovery efciency was very low, and a high concentration of
encrusted product on the wall of the drying camera occurred. Thus,
to perform this work, the lower temperatures (160/70 C) were selected. Atomizer pressures from 0.2 to 1 kg/cm2 were also tested,
and we found that when the nozzle pressure was 1 kg/cm2, the
drops were projected on the walls of the drying chamber with a
low recovery of powders. In contrast, when 0.4 kg/cm2 of pressure
was used, higher yields were obtained in the recovery of powders.
Suitable antioxidant activities were obtained when a blend of
GA and MD 20DE was used at a 1:1 ratio according to the preparation in Section 2.2.5. The NAEC (core) can be delivered by different
transport mechanisms through the layers of the encapsulating
materials that provide the structure for the capsules as well as
by aqueous solubilization of wall materials. The product obtained
has high antioxidant activity and carotenoids, so it could be used
in nutraceutical foods and possibly as a natural antimicrobial
(Careaga et al., 2003).
The non-extractable fraction of NAEC, which was evaluated as a
percentage of encapsulated NAEC, was between 90% and 91% for
microencapsulates of the three different non-aqueous extracts
(corn, sunower, and safower), and approximately 910% for
the extractable fraction of NAEC (Table 3). No signicant differences were found between the values of EE among the different extracts (p P 0.05). The amount of extractable oil depends on the
emulsion process, drying air temperatures, and physicochemical
characteristics of the wall material, which were kept constant. It
is possible that the content of saturated fatty acids induced different arrangements among the components of the wall materials
during microcapsule development. Another factor that affects the
content of non-encapsulated oil is the porosity of the wall material
and the method of extraction used. Drusch and Berg (2008) found
that the amount of non-encapsulated oil was slightly higher for
microencapsulation at drying temperatures (inlet/outlet) of 210/
90 C compared to 160/60 C. The EE was 8386% for the three
different encapsulates in relation to total carotenoid content (Table
3). The EE and extractable portion of NAEC and NAEC microcapsules was based on total carotenoid content (expressed as b-carotene) as the target chemical component.
Rocha et al. (2012) found that the EE of lycopene microencapsulation was 2129% using modied starch as the wall material.
Rodriguez-Huezo et al. (2004) reported that the microencapsulation efciency was between 25.6% and 87.5% for emulsions containing carotenoids using GA, gellan gum, and MD as wall
materials.
3.6. Stability tests for microencapsulates
The preservation of the antioxidant activity and water activity
of microencapsulated NAEC was evaluated after 60 d of storage,
which is the average time for consumption of a food powder, at
20 5 C (Davoodi et al., 2007). As shown in Table 4, the microcapsules retained approximately 72%, 68%, and 61% of the initial antioxidant activity for corn, sunower, and safower extracts,
respectively, after 60 d of storage. These results only represented
a loss of 8.5%, 12%, and 15% of the antioxidant activity, respectively,
compared to the original microencapsulated NAEC that was

35

evaluated at time zero. The yellow and red fractions as well as total
carotenoid content are shown in Table 4. Total carotenoid content
in the microencapsulated NAEC decreased by 22.1%, 22.7%, and
27.6% for NAEC prepared with corn, sunower, and safower oils,
respectively, during the storage period. The carotenoids from
microcapsules of NAEC prepared with corn oil had the highest antioxidant activity, which may be due to different fatty acid composition of the oils. Corn oil has a higher proportion (12.2%) of
saturated fatty acids compared to sunower (10%) and safower
(7.42%) oils, according to Mexican Standard References (NMX-F030-SCFI-2005; NMX-F-265-SCFI-2005; NMX-161-SCFI-2007),
which makes it less susceptible to degradation by oxidation. The
oxidation of fatty acids is a chain reaction due to various factors,
such as temperature, light, and the presence of metals. Once this
reaction is initiated in the fatty acids, it continues in the carotenoids (co-oxidation) (Takahashi et al., 2003). Saturated fatty acids
are more stable than polyunsaturated and monounsaturated fatty
acids, suggesting that carotenoids are oxidated more rapidly by
polyunsaturated oils than by monounsaturated oils, and much less
rapidly by saturated fatty acids. Therefore, the only way by which
carotenoids can undergo greater oxidation in oil containing more
saturated fatty acids is if the saturated oils were oxidated before
contacting the carotenoids (Omara-Alwala et al., 1985; Bezbradica
et al., 2005; Sachindra and Mahendrakar, 2005). Changes in antioxidant activity and total carotenoid content in the stored microcapsules could also be related to degradation reactions of lipids and
carotenoids by complex mechanisms of co-oxidation (Takahashi
et al., 2003) or to the presence of MD (D-glucose) and GA (that
has a protein portion), which may trigger the Maillard reaction that
usually occurs during food processing and storage (Pitalua et al.,
2010).
Corn oil has good oxidative stability, which is partially attributed to the nonrandom distribution of fatty acids on triglycerides.
It has been determined that 98% of the fatty acids esteried in the
sn-2 position of corn oil triglycerides are unsaturated, leaving the
outer sn-1 and sn-3 positions with possibilities of binding saturated fatty acids and the unsaturated acids that may still be present
in the oil. Therefore, since the outer positions of the triglycerides
are more reactive, the polyunsaturated fatty acids in the sn-2 position present a certain degree of protection from oxidation (OBrien,
2004).
The extractable fraction of the oil phase, which has greater
exposure to oxygen, was more susceptible to the oxidation processes than the encapsulated fraction (Shimada et al., 1991;
Velasco et al., 2000) which is less exposed to oxygen, in the NAEC
microcapsules prepared with sunower and safower oils. The
opposite was observed for microcapsules prepared with corn oil,
even though a similar percentage of non-encapsulated oil was
present for the three types of NAEC microcapsules. This observation could be due to the above mentioned lower proportion of
unsaturated fatty acids present in corn oil compared with sunower and safower oils.
The loss of antioxidant activity and total carotenoid content of
the microencapsulates may be directly related to the amount of
extractable or non-encapsulated oil containing carotenoids in the
microcapsules, which is exposed to oxygen and causes oxidation
of carotenoids. In addition, the presence of open pores in the wall
of microcapsules allows accessibility of oxygen to NAEC structures.
Mrquez-Ruiz et al. (2003) reported that the extractable oil fraction in matrices containing an oily phase is affected by numerous
variables, but in some cases, the extractable oil was more prone
to oxidation than the non-extractable fraction.
The delivery and controlled release of carotenoids from microcapsules are decisive in understanding the effects of the active
agent for a particular application and impact their availability.
The release of bioactives from capsules is affected by the chemical

36

A.Y. Guadarrama-Lezama et al. / Journal of Food Engineering 112 (2012) 2937

Table 4
Characteristics of NAEC microcapsules after storage for 60 d at 20 5 C.
Corn
a

Antioxidant activity (%)

Red fraction (CR)b
Yellow fraction (CY)b
Total carotenoid content as
b-carotene (lg/mL)
Water activity (aw)
Moisture content (%)

Sunower
a

72.0 0.8
59.2 0.1c
96.8 1.2d
156.0 3.9g
0.17 0.01l
3.06 0.3m

Safower
a

68.1 2.2
54.3 0.03c
89.3 0.5e
143.6 0.1h

61.3 3.4b
51.3 0.04c
75.9 0.5f
127.2 1.0i

0.18 0.01l
5.50 0.2n

0.15 0.0l
5.02 0.07n

Statistical analysis was performed by the type of oil used for extraction, and different letters indicate a signicant difference at p 6 0.05.
a
Values based on the antioxidant activity with respect to the non-aqueous
extracts.
b
Isochromatic families are CR: capsanthin and capsorubin; CY: zeaxanthin,
b-cryptoxanthin, and b-carotene expressed as lg/mL of extract.

structure of the wall materials and active agent, concentration of

encapsulated antioxidant, environmental conditions (temperature,
pH, and release media), and particle size and its morphology (Lee
and Ying, 2008). Active compounds with antioxidant activity, such
as the non-aqueous extracts of Capsicum, may be of potential application in the food industry; however, their use depends on the release mechanism. One of the methods for achieving controlled
release in foods is microencapsulation, which has been reported
to release the active agent by diffusion, biodegradation, swelling,
or osmotic pressure (Pothakamury and Barbosa-Cnovas, 1995;
Sabliov and Astete, 2008). The release of microencapsulated NAEC
can occur by a diffusion process through the polymeric material as
well as solubilization of wall material; however, application of this
technology would depend on the specic use or consumption of
the microcapsules (Lee and Ying, 2008).
4. Conclusions
In this study, we obtained non-aqueous extracts of Capsicum
with high antioxidant activity by using edible vegetable oils as
extraction media, thus avoiding the use of volatile solvents that
are potentially harmful to the environment. Corn oil provided the
highest yields during the extraction, and the microcapsules obtained with this oil were the most stable. The encapsulation of
non-aqueous extracts by spray-drying allowed for the protection
of active agents of the extracts against oxidative and deterioration
processes. Approximately 80% of the antioxidant activity of the
non-aqueous extracts was preserved in the microencapsulates.
The microcapsules did not contain fractures, and this nding may
have contributed to the protective action against oxidation. The
microcapsules obtained could be included as functional ingredients in a diverse range of food products and may have utility as
a possible natural antimicrobial agent.
Acknowledgements
The authors thank the nancial support for this work from the
National Polytechnic Institute (IPN-Mexico) through the Projects
SIP 20121026, SIP 20121754, and the PIFI Program as well as from
the Institute of Science and Technology of Mexico Citys Government (ICYTDF) through the Project PICS08-15. Author GuadarramaLezama received a study grant from the Mexican National Council
for Science and Technology (CONACYT).
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