Food Chemistry 114 (2009) 616–622

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Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem

Microencapsulation by spray drying of bioactive compounds from

cactus pear (Opuntia ficus-indica)
Carmen Saénz a,*, Sandra Tapia a, Jorge Chávez c, Paz Robert b
a
Departamento de Agroindustria y Enología, Facultad de Ciencias Agronómicas, Universidad de Chile, Casilla 1004, Santiago, Chile
b
Depto. Ciencia de los Alimentos y Tecnología Química, Facultad de Ciencias Químicas y Farmacéuticas, Universidad de Chile, Casilla 133, Santiago, Chile
c
Depto. Tecnología Farmacéutica, Facultad de Ciencias Químicas y Farmacéuticas, Universidad de Chile, Casilla 133, Santiago, Chile

a r t i c l e i n f o a b s t r a c t

Article history: Bioactive compounds of pulp (CP) and ethanolic (CE) extracts of the cactus pear (Opuntia ficus-indica)
Received 14 May 2008 were encapsulated with maltodextrin (MD) or inulin (I). A 22 statistical factorial design was then used
Received in revised form 19 August 2008 to study the stability of the powders obtained at the optimal conditions for each system (CP–MD, CP–I,
Accepted 30 September 2008
CE–MD and CE–I) at 60 °C in the dark. The 3:1 ratio of core/coating material and 140 °C inlet air temper-
ature were the optimal conditions for CP–MD and CE–MD systems; whereas, for CP–I and CE–I, the ratios
were 3:1 and 5:1, respectively, and 120 °C was used for the inlet air temperature for both systems. An
Keywords:
increase of phenolic compounds was observed in all systems during storage at 60 °C. Indicaxanthins in
Cactus pear
Spray-drying
all systems showed a slow degradation during storage at 60 °C and were more stable than betacyanins.
Microencapsulation The microcapsules described in this study represent an interesting food additive for incorporation into
Betalains functional foods, due to both the presence of antioxidants and as a red colourant.
Polyphenols Ó 2008 Elsevier Ltd. All rights reserved.
Stability

1. Introduction
Cactus pear (Opuntia spp.) is a tropical fruit tree, native to
America, which grows in arid and semiarid regions (Pimienta-Bar-
rios & del Castillo, 2002). There are green fruits and also coloured
fruits (red, yellow or purple) due to the presence of various pig-
ments such as betalains and carotenes (Castellar, Obon, & Fernán-
dez-López, 2006; Díaz, Santos, Kerstupp, Villagómez, & Scheivar,
2006; Tesoriere, Fazzari, Allegra, & Livrea, 2005).
Cactus pear is one of the few sources of betalains in nature and
therefore presents itself as an attractive alternative to replace syn-
thetic additives; this is in addition to the advantages of production
of the fruit for direct consumption. Cactus pear could have a double
application, both becoming an option for obtaining natural colour-
ing features and providing health benefits through its antioxidant
function (Stintzing & Carle, 2004; Tesoriere et al., 2005).
The literature reports few scientific studies regarding the pres-
ence of phenols or other antioxidant compounds in cactus pear
fruits. The purple cultivar has the highest concentration of total
phenols, at approximately 660 mg/l juice (Stintzing et al., 2005).
Other studies have identified the presence of flavonoids as flavonol
glycosides, amongst which significant amounts of isorhamnetin-3-
rutinoside, rutin and kaempferol-3-rutinoside were found in a
* Corresponding author. Tel.: +56 2 9785731; fax: 56 2 9785796.
E-mail address: csaenz@chile.cl (C. Saénz).
blend of yellow and red cultivars (Galati et al., 2003). The intake
of polyphenols has been inversely correlated to the incidence of
several chronic diseases, such as several types of cancer and car-
diovascular disease (Mertens-Talcott, Zadezensky, De Castro,
Derendorf, & Butterweck, 2006).
The stability of betalains has been studied by several research-
ers, and it has been shown that they are affected by pH, water
activity, exposure to light, oxygen, temperature and enzymatic
activities; moreover, temperature is the most decisive factor for
betalain decomposition (Castellar, Obon, Alacid, & Fernández-
López, 2003). The stability is an important aspect to consider for
use of these pigments as antioxidants and colourants in foods.
The stabilization of betalains and polyphenols could be im-
proved using microencapsulation technologies, such as spray dry-
ing (Desai & Park, 2005), for use in industrial purposes and to
ensure its bioavailability. Microencapsulation is described as a
technique wherein a bioactive compound is encapsulated by a bio-
polymer, thereby protecting it from oxygen, water or other condi-
tions to improve its stability (Desai & Park, 2005). This method is
also used to change liquid solutions to powders, which are easier
to handle. Rodríguez-Hernández, González-García, Grajales-Lagun-
es, Ruiz-Cabrera, and Abud-Archila (2005) studied spray drying as
a technique for stabilizing cactus pear pulp from Opuntia
streptacantha.
Different types of encapsulating agents have been used for spray
drying; these include polysaccharides (starches, maltodextrins,

0308-8146/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.foodchem.2008.09.095
 C. Saénz et al. / Food Chemistry 114 (2009) 616–622
corn syrups and arabic gum), lipids (stearic acid, mono and digly-
cerides), and proteins (gelatin, casein, milk serum, soy and wheat)
(Gibbs, Kermasha, Alli, & Mulligan, 1999). The most commonly
used materials for microencapsulation are maltodextrins of differ-
ent dextrose equivalents. Maltodextrins are obtained by acid
hydrolysis of several starches (corn, potato or others). In general,
maltodextrins have high solubility in water, low viscosity, bland
flavour and colourless solutions (Gibbs et al., 1999) and are exten-
sively used in the food industry.
An interesting possible encapsulation agent may be inulin, due
to its technical and nutritive properties (Stevens, Meriggi, & Booten,
2001). Inulin is a fructooligosaccharide (FOS) obtained commer-
cially from chicory (Cichorium intybus) root, Dahlia (Dahlia pinuata
Cav.) and Jerusalem artichoke (Helianthus tuberosus); they have an
average polymerisation degree (DP) of 10–14, 20 and 6, respec-
tively. The inulin is composed of fructose units with b (2-1) links
with glucose at the end of the chain. Inulin shows prebiotic effects
and dietary fibre action and improves calcium biodisponibility,
amongst other benefits. Inulin is only hydrolysed in small amounts
in the stomach and the large intestine without the formation of
monosaccharides; it is fermented by the large intestinal microflora
into short chain fatty acids, lactic acid and gas. Therefore, there is no
resultant increase to the glycemic index, which is important as a
potential ingredient for diabetic foods (Stevens et al., 2001).
The objective of this research was to study the effect of inlet air
temperature and the ratio of the bioactive cactus pear compound
to the encapsulating agent on the betalain and polyphenol yields
using spray drying, and the stability of the powders obtained.
2. Material and methods
2.1. Materials
Cactus pear fruits (Opuntia ficus-indica) were obtained from a
plantation located in the Antumapu Experimental Station that be-
longs to the University of Chile, Santiago, Chile. Maltodextrin (MD)
GlobeÒ, INDUCORN (DE = 10) and inulin RaftilinaÒ (I) HP (DP > 23)
were used. All other reagents were of analytical grade.
2.2. Pulp and ethanolic extract preparation
The fruits (13.75 kg) were manually peeled after washing and
pulped in an Alexanderwerk screw press with a 2 mm screen,
obtaining 11 kg of pulp. The pulp was packed in polypropylene
bags and frozen at 20 °C.
Ethanolic extract preparation: 1 kg of pulp was macerated with
ethanol and water (1:1) during a total of 14 h. Three extractions were
made until the pulp was light red. Extracts were combined and con-
centrated in a Buchi RE120 evaporator at 45 °C until reaching the
same soluble contents of the pulp, obtaining 0.46 kg of extract. The
extract was packed in polypropylene bags and frozen at 20 °C.
2.3. Preparation of the microcapsules
Encapsulation in both maltodextrin and inulin were prepared as
follows: cactus pear pulp (30 g) or ethanol extract (15 g) was
mixed with maltodextrin (6–30%) or inulin (3–15%) with constant
stirring. The maltodextrin was previously swollen in distilled
water for 12 h. In the case of inulin, it was heated at 60 °C prior
to the addition of the pulp or extract. Each preparation was homog-
enised with an Ultraturrac IKA T50 homogenizer at 4000 rpm for
5 min. The resultant solutions were fed to a Buchi B-191 spray-
dryer (Switzerland). The spray-dryer was operated at inlet temper-
ature ranging from 140–160 ± 5 °C to 120–160 ± 5 °C for MD and I,
respectively. The air flow, rate of feeding and atomization pressure
617
were 600 l/h, 10 ml/min and 20 psi, respectively, for both encapsu-
lating agents. The powders obtained were stored to exclude light
and were kept at 20 °C until analysed.
2.4. Cactus pear pulp and ethanolic extract analysis
Moisture content, soluble solids (°Brix), pH and acidity were
determined according to AOAC (1996) methods. The total sugars
were determined by the Antrona method (Osborne & Voogt,
1986) in an UNICAM UV/VIS spectrometer UV3.
The total phenolic content was determined according to the Fo-
lin–Ciocalteau method (Bordeau & Scarpa, 2000), and the results
were expressed as gallic acid equivalents according to a calibration
curve (133.8–428.0 lg/ml; r2 = 0.9901). Analyses of the phenolic
compounds were carried out in duplicate and averaged.
The betalains analyses were performed spectrophotometrically
according to the methods of Stintzing et al. (2005). Betacyanins
pigments were monitored at 535 nm, and indicaxanthin was mon-
itored at 484 nm. The identification was performed by HPLC using
a Merck Hitachi L6200 pump, a Waters 996 photodiode-array
detector, and a C18 column (5 lm  4.6 mm i.d.  25 cm, YMC).
The mobile phases used were solvent A (1% acetic acid in water)
and solvent B (1% acetic acid in acetonitrile) according to a pro-
gram described by Fernández-López and Almela (2001).
Vitamin C was determined by HPLC (Straten & Claessens, 2004)
using an Agilent G1311A pump, an Agilent G1315B diode array, a
Zorbac SB-Aq column (5 lm  4.6 mm i.d.  150 mm, Agilent),
and a phosphate:acetonitrile (90:10) buffer as the mobile phase.
Antioxidant activity was evaluated in accordance with the
DPPH method (Kukoski et al., 2005). The results were expressed
as TROLOX equivalent activity (TEAC).
Colour parameters (L*, a*, b*) were determined with a MINOLTA
CR-200b equipment. The Hue angle (h° = tan1(b*/a*) and the Chro-
ma C* value were calculated according to McGuire (1992).
2.5. Microcapsule powder analysis
2.5.1. Total bioactive compounds
The total phenolic and betalains compounds were determined
following the methods of Barbosa, Borsarelli, and Mercadante
(2005) and Yoo, Song, Chang, and Gyu-Lee (2006), respectively,
with some modifications. One hundred milligrams of the prepared
microcapsules were accurately weighed and dispersed in 1 ml eth-
anol, acetic acid, and water (50:8:42). This dispersion was agitated
using a Vortex (1 min) and then an ultrasonicator twice for 20 min.
The supernatant was centrifuged at 112,896g for 5 min and then
filtered. The amounts of phenolic and betalains compounds were
quantified by the Folin–Ciocalteau and Stintzing et al. (2005)
methods, respectively.
2.5.2. Surface betalains and surface phenolic compounds
For the determination of surface betalains and surface phenolic
compounds, 100 mg of microcapsules were treated with 10 and
1 ml of a mix of ethanol and methanol (1:1), respectively. These
dispersions were agitated in a Vortex at room temperature for
1 min and then filtered (0.45 lm Millipore filter). The amounts of
phenolic and betalains compounds were quantified by the Folin–
Ciocalteau (Bordeau & Scarpa, 2000) and Stintzing et al. (2005)
methods, respectively. The surface bioactive compounds percent-
age (SB) and bioactive compounds microencapsulated yield
(BMY) were calculated according to Eqs. (1) and (2), respectively
surface bioactive compounds
SBð%Þ ¼  100; ð1Þ
theoretical total bioactive compounds
BMYð%Þ ¼ 100  SBð%Þ: ð2Þ
618 C. Saénz et al. / Food Chemistry 114 (2009) 616–622

2.5.3. Moisture determination Table 1

Moisture determination was performed according to AOAC Physical and chemical characteristics of pulp (CP) and ethanolic extract (CE) from
cactus pear.
method (1996).
CP CE
2.5.4. Scanning electron microscopy (SEM) Total soluble solids (°Brix) 14.00 ± 0.00 14.53 ± 0.06
The outer structures of the microencapsules obtained by opti- Total sugars (%) 15.02 ± 0.22 17.42 ± 0.28
mal conditions were studied by SEM. The samples were coated pH 5.63 ± 0.06 5.57 ± 0.04
Acidity (% citric acid) 0.037 ± 0.001 0.119 ± 0.007
with gold/palladium using a Varian Vacuum Evaporator PS 10E Moisture content (%) 85.32 ± 0.03 –
and analyzed using a JEOL JSM-25SII (Jeol, Tokyo, Japan) scanning
Colour parameters
electron microscope operated at 30 kV. The images were obtained L* (lightness–darkness) 21.3 ± 0.20 20.33 ± 0.06
with a Mamiya Roll Film Holder camera (Model 2) coupled to the a* (redness–greenness) 2.43 ± 0.31 1.10 ± 0.35
microscope using Kodak 120 T-Max ISO 100 film. b* (blueness–yellowness) 1.17 ± 0.06 1.10 ± 0.17
h° (hue) 25.82 ± 3.4 45.85 ± 5.44
C* (chroma) 2.7 ± 0.27 1.56 ± 0.36
2.6. Accelerated storage stability test
Betacyanins (BE/100 g) 28.09 ± 0.17 21.54 ± 0.22
Betaxanthins (IE/100 g) 9.96 ± 0.10 10.21 ± 0.08
Microcapsules obtained under optimal conditions (CP–MD, CP–
Total phenolics compounds (mg GAE/l) 909.47 ± 29.34 777.14 ± 4.04
I, CE–MD and CE–I) were stored at 60 °C in a forced-air oven with Vitamin C (mg/100 g) 1.69 ± 0.05 nd
controlled temperature and in the absence of light for 44 days. Antioxidant activity (mmol TEAC/g) 3.3 2.87
Samples of 0.1 g of each powder were transferred to
Abbreviations: CP, cactus pulp; CE, cactus ethanolic extract; BE, betanin equivalent;
450  250 mm clear glass vials. For determination of bioactive IE, indicaxanthin equivalent; GAE, gallic acid equivalent; nd, non-detected.
compounds, duplicate vials were removed every 4 days during
the first 20 days and then every 8 days until the study was
completed. respectively. The betalain content is affected by factors such as cul-
tivar or variety, stage of maturity and climate or geographic site of
2.7. Statistical design production (Stintzing & Carle, 2004).
The CP total phenolic content was higher than that reported by
The experiments were performed with a 22 central composed Stintzing et al. (2005) of 660 mg/l and by Morales (2007) of
experimental design constituted by 10 experiments for each 777.4 mg/l. The CE showed a lower total phenolic content com-
encapsulating agent. The independent variables considered were pared with the CP. Similar content was found in grapes (50–
the temperature of drying (140–160 and 120–160 °C for MD and 490 mg/100 g fresh matter), and lower values were reported for
I, respectively) and the ratio of core material to coating material blackcurrant (140–1200 mg/100 g fresh matter) and for blueberry
(1:1–5:1 for both MD and I). The dependent variables were the effi- (135–280 mg/100 g fresh matter) (Bravo, 1998). The identified bet-
ciency of betalains and total phenolic microencapsulation. The re- alains in CP are shown in the chromatograms (Fig. 1A and B) at dif-
sponse surface methodology was applied to optimise the ferent wavelength. In both figures, peaks 1 and 2 correspond to
encapsulation yield of bioactive compounds using Statgraphics betacyanins (betanin and isobetanin, respectively) and peak 3 to
software version 7.0 (Manugistics Inc., Statistical Graphics betaxanthins (indicaxanthin), in agreement with Fernández-López
Corporation, 1993, Rockville, MA). and Almela (2001). Similar behaviour was observed in CE.
Vitamin C was found in CP (1.69 mg/100 g), but none was de-
tected in CE, suggesting that vitamin C was lost during the ethanol
3. Results and discussion extract preparation steps involved. The content of vitamin C has
been reported previously with values ranging between 1 and
3.1. Pulp and extract characteristics and bioactive compounds 41 mg/100 g (Feugang, Konarski, Stintzing, & Zou, 2006; Sáenz &
Sepúlveda, 2001; Stintzing et al., 2005; Tesoriere et al., 2005).
Table 1 shows the physical and chemical characteristics of the The antioxidant activities were 3.30 lmol TEAC/g and
pulp (CP) and ethanolic extract (CE) from the cactus pear. The pulp 2.87 lmol TEAC/g for CP and CE, respectively. Butera et al. (2002)
results, as related to the fruit ripeness, are similar to those of other found 4.20 lmol TEAC/g in red cactus pear pulp, and Stintzing
studies, where the values of the sugar content ranged between 10% et al. (2005) reported 3.64 lmol TEAC/g with another method. This
and 17% (Sáenz & Sepúlveda, 2001). In CE, the total sugar was antioxidant activity is similar to those reported for other fruits,
slightly higher (17.42%) due to the concentration of those compo- such as pineapple, passion fruit and blackberry (Kukoski, Asuero,
nents during the extract preparation. The soluble solid contents Troncoso, Mancini-Filho, & Fett, 2005). The lower antioxidant
were similar in both CP and CE; similar behaviour using different activity in CE as compared to CP corresponds to the lower content
ethanol and water extraction solvents was reported by Castellar of bioactive components found in the extract.
et al. (2006), and similar values were determined by Sáenz and
Sepúlveda (2001). The pulp acidity and pH were similar to those 3.2. Optimization of cactus pear bioactive compound
reported by other authors, who reported the acidity to be 0.03– microencapsulation by response surface methodology
0.18% expressed as citric acid (Morales, 2007) with a pH of 5.3–
7.1 (Castellar et al., 2003; Morales, 2007; Sáenz & Sepúlveda, The encapsulation yields of betacyanin, indicaxanthin and poly-
2001). The CP colour (a*) was higher than that of CE, due to a great- phenols (BMY) in CP–MD microcapsules were in the ranges from
er betacyanin content (Table 1), suggesting lower betacyanin 98.40 to 99.49, 91.16 to 97.67 and 39.41 to 74.78, respectively.
extraction during the preparation of CE. Castellar et al. (2006) ob- The CP–I microcapsules had ranges from 98.19 to 99.42, 92.74 to
served that the betanin extraction fell with increasing ethanol 98.50 and 45.93 to 78.37, respectively. The CE–MD microcapsules
concentrations. were in the range from 99.16 to 99.56, 96.97 to 98.33 and 49.71
The betacyanin and betaxanthin contents from CP were lower to 80.79, respectively. The CE–I microcapsules were in the range
than those reported by Stintzing et al. (2005), 41.05 mg/100 g from 98.34 to 99.54, 95.11 to 98.39 and 22.98 to 74.86, respec-
and 18.65 mg/100 g, respectively, and greater than those reported tively. In general, the betacyanin and indicaxanthin encapsulation
by Morales (2007), 11.10 mg/100 g and 2.93 mg/100 g, yields (BMY) reached values above 98% and 92%, respectively.
 C. Saénz et al. / Food Chemistry 114 (2009) 616–622
Fig. 1. Chromatograms of cactus pear betalains determined by HPLC. Betanin (1), isobetanin (2) and indicaxanthin (3).
When MD was used, Desobry, Netto, and Labuza (1997) and Loksu-
wan (2007) found b-carotene microencapsulation yields of 47% and
62%, respectively, and Barbosa et al. (2005) reported a 54% bixin
microencapsulation yield.
The phenolic compound encapsulation yield showed a greater
variation than the other bioactive compounds, with values ranging
from 23% to 81%. The response surface methodology was applied to
optimise the encapsulation yields of betacyanin, indicaxanthin and
polyphenols. The desirability function approach is a method that
assigns a score (between 0 and 1) to a set of responses and chooses
factors that maximise that score (1 representing a completely
desirable value, such as 100% encapsulation of each one of the bio-
active components). Fig. 2A–D shows the graphs obtained with the
response surface methodology for the CE–I, CE–MD, CP–I, CP–MD
designs, respectively. The temperature had no significant
(p > 0.05) effect on the betalains and polyphenols encapsulation
yields, except in the case of the CP–MD system. The CP or CE/
encapsulating agent ratio was significant (p < 0.05) for polyphenols
encapsulation yield in all the systems studied and betalains encap-
sulation yield was only significant in the case of CP–MD. The opti-
mal conditions were 140 °C and 3:1 ratio of core material to
coating material, when using MD encapsulating agent. It could be
pointed out that the 1:1 and 5:1 MD systems have different water
(40% and 64%, respectively) and solid contents (34.2% and 10.2%,
respectively). The 3:1 MD system, corresponding to the optimal
condition, was similar to the 5:1 system in the water content but
with a 14.2% solid content, suggesting that the core/coating/water
ratio may affect the encapsulation yields or that the interaction be-
tween the bioactive compounds and the coating material could be
more important. The same behaviour was observed in the case of
inulin, where 120 °C and 3:1 ratio of core material to coating mate-
rial for CP and 120 °C and 5:1 ratio of core material to coating
material for CE, were the optimal conditions, showing that the CP
619
mucilage could aid the drying process, being enough at a lower
encapsulating agent proportion.
3.3. Microcapsule powder obtained under optimal conditions
Table 2 shows the concentration values of bioactive compounds
of pulp and ethanol extract before and after encapsulation. The
recovery of betacyanins and indicaxanthins in the pulp with MD
and I was 100%, showing that the drying temperature and the type
of encapsulating agent did not affect the recovery of the bioactive
compound. In the ethanol extract, the recoveries of betacyanins
and indicaxanthins were lower in MD at 62% and 67%, respectively,
and in I at 81% and 86%, respectively. The higher degradation in MD
of bioactive compounds could be attributed at the high inlet air
temperature (140 °C) used. As can be seen in Table 2, the microen-
capsulated pulp showed a higher recovery than the microencapsu-
lated ethanol extracts, suggesting that components of the pulp
(mucilage and fiber) help the encapsulating process. In the pure
b-carotene encapsulated with 25 DE maltodextrin, losses of 11%
were obtained (Desobry et al., 1997). The recoveries of polyphenols
were over 100%, which could be a consequence of the hydrolysis of
the cactus pear polyphenol conjugates during the preparation of
the samples or during the drying process (Turkmen, Sari, & Velio-
glu, 2005). Table 3 shows the characterisation of pulp and etha-
nolic extract of cactus pear microcapsules obtained under
optimal conditions with MD and I.
Fig. 3A–D presents scanning electron microscopic photographs
of microcapsules for the CP–MD, CP–I, CE–MD and CE–I designs,
respectively. The morphology of microcapsules with both encapsu-
lating agents was irregularly spherical in shape with an extensively
dented surface. The formation of the dented surfaces of the spray-
dried particles was attributed to the shrinkage of the particles
during the drying process. Similar morphology was observed in
620 C. Saénz et al. / Food Chemistry 114 (2009) 616–622

Fig. 2. Graphs obtained by response surface methodology for the CE–I (A), CE–MD (B), CP–MD (C) and CP–I (D) designs, respectively.

Table 2 Table 3
Concentration values of bioactive compounds of cactus pear pulp and ethanolic Characterisation of pulp and ethanolic extract of cactus pear microcapsules obtained
extract before and after encapsulation. by optimal conditions with maltodextrin and inulin.
System Betacyanins Indicaxanthins Polyphenols CP–MD CP–I CE–MD CE–I
(mg BE/g (mg IE/g powder) (mg GAE/g
powder) powder) Moisture content (%) 2.21 ± 0.26 4.11 ± 0.12 2.39 ± 0.01 5.12 ± 0.12

CP–MD Before spray-drying a

0.58 0.21 1794 Colour parameters
After spray drying 0.6 ± 6  103 0.22 ± 1  103 2135 ± 0.0 L* (lightness–darkness) 65.6 ± 1.75 69.7 ± 1.16 76.0 ± 1.54 69.3 ± 0.8
Recovery (%) 100 100 119 a* (redness–greenness) 34.7 ± 0.26 32.3 ± 0.98 24.4 ± 0.67 28,2 ± 0,70
b* (blueness– 8.23 ± 0.29 8.83 ± 0.15 2.13 ± 0.15 3.13 ± 0.06
CP–I Before spray-dryinga 0.58 0.22 1802 yellowness)
After spray drying 0.64 ± 9  103 0.24 ± 2  103 2028 ± 4.5 h° (hue) 346.6 ± 0.4 344.7 ± 0.30 355.0 ± 0,26 353.7 ± 0.18
Recovery (%) 100 100 112 C* (chroma) 35.7 ± 0.30 33.5 ± 0.98 24.5 ± 0.67 28.4 ± 0.70
CE–MD Before spray-dryinga 0.45 0.21 1607 Antioxidant activity 34.0 ± 1.23 24.0 ± 1.23 19.2 ± 0.51 61.7 ± 2.24
After spray drying 0.28 ± 3  103 0.14 ± 4  103 1812 ± 5.4 (mmol TEAC/g)
Recovery 62 67 112 DPPH (IC50/mg/l) 18.9 ± 0.68 27.15 ± 1.09 33.3 ± 0.88 10.4 ± 0.38

CE–I Before spray-dryinga 0.62 0.29 2223 Abbreviations: CP, cactus pulp; CE, cactus ethanolic extract; BE, betanin equivalent;
After spray drying 0.50 ± 7  103 0.25 ± 5  103 2410 ± 10 IE, indicaxanthin equivalent; GAE, gallic acid equivalent; MD, maltodextrin; I,
Recovery 81 86 108 inulin.

Abbreviations: CP, cactus pulp; CE, cactus ethanolic extract; BE, betanin equivalent;
IE, indicaxanthin equivalent; GAE, gallic acid equivalent; MD, maltodextrin; I,
inulin.
a
Calculated according to polyphenols pulp content.
microcapsules of other cactus pear cultivars (Opuntia lasiachanta)
pigments with maltodextrin (10DE) (Díaz et al., 2006), of Amaran-
thus (Cai & Corke, 2000) using maltodextrin of different dextrose
equivalents (10DE; 20–23DE and 28–31DE), and of b-carotene,
using modified tapioca starch and maltodextrin (24DE) as encapsu-
lating agents (Loksuwan, 2007). Nevertheless, smooth spheres
have primarily been observed in microcapsules of black carrot pig-
ments (Daucuscarota L.) with maltodextrin (10DE and 20–23DE)
(Ersus & Yurdagel, 2007).
3.4. Storage stability evaluation
The evolution of betacyanin, betaxanthin and polyphenol con-
tents from CP–MD, CP–I, CE–MD and CE–I microcapsules obtained
with the optimal conditions and storage at 60 °C is shown in
Table 4.
Fig. 4 shows the natural log of the percentage retention vs. time
(days) for betacyanins in CP–MD, CP–I, CE–MD and CE–I curves at
60 °C. The degradation kinetics of betacyanins initially followed a
pseudo-first order behaviour, in microcapsules of CE with MD or
I, corresponding to superficial (SB) betacyanins degradation. The
second slope represented a second pseudo-first order step with a
slower rate than the first slope, corresponding to the internal beta-
cyanins degradation. Only one slope (pseudo-first order) was ob-
served when CP was encapsulated with MD or I, suggesting that
the degradation of superficial and internal betacyanins occurred
at the same rate. As was mentioned above, mucilage could play a
role in this behaviour.
Previous research has shown that the degradation of anthocya-
nins encapsulated in MD of different DEs (Ersus & Yurdagel, 2007)
follows first order kinetics during the storage. Table 5 shows the
pseudo-first order betacyanins degradation rate constant (kobs) ob-
tained from the slopes of the logarithmic plots of the percentage
retention vs. time (days). The betacyanins degradation rate in CP
microcapsules occurred at the same rate (p > 0.05) in both encap-
sulating agents, whereas in CE was significantly lower (p < 0.05)
in I than in MD, showing better performance of inulin. Indicaxan-
thin in all systems studied showed a slow degradation during stor-
age at 60 °C and more stability than betacyanin. On the other hand,
 C. Saénz et al. / Food Chemistry 114 (2009) 616–622 621

Fig. 3. Scanning electron microscopic photographs of microcapsules for the CP–MD (A), CP–I (B), CE–MD (C) and CE–I (D) designs, respectively.

Table 4
Evolution of betacyanin, indicaxanthin and polyphenol contents from CP–MD, CP–I, CE–MD and CE–I microcapsules obtained under optimal conditions and stored at 60 °C.

System Compound Time (days)

0 4 8 12 16 20 28 36 44
Pulp/MD Betacynin (mg/g) 0.60 0.57 0.54 0.52 0.50 0.47 0.42 0.40 0.38
Pulp/I 0.64 0.59 0.59 0.54 0.53 0.52 0.46 0.43 0.38
Extract/MD 0.28 0.28 0.25 0.22 0.22 0.22 0.19 0.17 0.15
Extract/ I 0.50 0.44 0.40 0.38 0.35 0.35 0.35 0.32 0.30
Pulp/MD Indicaxanthin (mg/g) 0.22 0.22 0.2 0.19 0.19 0.19 0.16 0.16 0.16
Pulp/I 0.24 0.22 0.22 0.20 0.20 0.20 0.19 0.18 0.15
Extract/MD 0.14 0.15 0.13 0.13 0.12 0.13 0.13 0.12 0.07
Extract/I 0.25 0.23 0.22 0.21 0.20 0.21 0.21 0.20 0.20
Pulp/MD Polyphenol (mg/g) 2.28 2.32 2.31 2.35 2.44 2.51 2.17 2.31 2.01
Pulp/I 2.26 2.44 2.52 2.62 2.62 2.76 2.12 2.95 3.00
Extract/MD 1.81 1.75 1.70 1.69 1.67 1.65 1.61 1.58 1.41
Extract/I 2.41 2.98 3.05 3.33 3.35 3.65 3.57 3.57 3.81

an increase of phenolic compounds was observed in CP–MD, CP–I,

CE–MD and CE–I during storage at 60 °C.
In conclusion, the CP microcapsules obtained with the optimal
conditions showed a higher recovery of bioactive compounds in
the drying process. The effect of encapsulating agent on the beta-
cyanins degradation rate was observed in CE microcapsules but
not in CP microcapsules, suggesting that the other pulp compo-
nents (as mucilages) play a role on the encapsulating process.

Table 5
Betacyanins degradation rate constant at 60 °C of CP–MD, CP–I, CE–MD and CE–I
microcapsules obtained under optimal conditions.

System k(obs) (days1)/superficial k(obs) (days1)/internal r2

2 4(a)
CP–MD 1.06  10 ± 1.93  10 0.990
CP–I 1.07  102 ± 1.63  104(a) 0.989
2 4
CE–MD 7.84  10 ± 2.42  10 1.28  102 ± 2.84  105(b) 0.992
CE–I 3.07  102 ± 9.26  105 0.58  102 ± 1.11  104(c) 0.948

Fig. 4. Percentage retention vs. time (days) for betacyanins in CP–MD (s), CP–I (j), Values were obtained from plots of the slopes of ln (%retention) vs. time. Different
CE–MDsup (N), CE–MD (4), CE–Isup (), CE–I (}), at 60 °C. letters show significantly different between systems (p < 0.05).
622 C. Saénz et al. / Food Chemistry 114 (2009) 616–622
The cactus pear microcapsules described in this study represent a
promising food additive for incorporation into functional foods,
due to both antioxidant content and potential as a red colourant.
Acknowledgements
This work is part of MULT 06/26-2 project (Departamento de
Investigación y Desarrollo of Universidad de Chile) and 17/07-08,
CSIC-Universidad de Chile project.
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