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International Journal of Food Properties

ISSN: 1094-2912 (Print) 1532-2386 (Online) Journal homepage: https://www.tandfonline.com/loi/ljfp20

Characterization and stability of pitaya pearls


from hydrocolloids by reverse spherification

Siti Fatimah Azzahra Bubin, Solihah Mat Ali, Radhiah Shukri, Wan Zunairah
Wan Ibadullah, Nurul Shazini Ramli, Nor Afizah Mustapha & Ismail Fitry
Mohammad Rashedi

To cite this article: Siti Fatimah Azzahra Bubin, Solihah Mat Ali, Radhiah Shukri, Wan Zunairah
Wan Ibadullah, Nurul Shazini Ramli, Nor Afizah Mustapha & Ismail Fitry Mohammad Rashedi
(2019) Characterization and stability of pitaya pearls from hydrocolloids by reverse spherification,
International Journal of Food Properties, 22:1, 1353-1364, DOI: 10.1080/10942912.2019.1647234

To link to this article: https://doi.org/10.1080/10942912.2019.1647234

© 2019 Siti Fatimah Azzahra Bubina, Solihah


Mat Alia, Radhiah Shukria, Wan Zunairah
Wan Ibadullahb, Nurul Shazini Ramlib,
Nor Afizah Mustaphaa and Ismail Fitry
Mohammad Rashedia. Published with
license by Taylor & Francis Group, LLC

Published online: 05 Aug 2019.

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INTERNATIONAL JOURNAL OF FOOD PROPERTIES
2019, VOL. 22, NO. 1, 1353–1364
https://doi.org/10.1080/10942912.2019.1647234

Characterization and stability of pitaya pearls from hydrocolloids


by reverse spherification
Siti Fatimah Azzahra Bubina, Solihah Mat Alia, Radhiah Shukria, Wan Zunairah Wan Ibadullahb,
Nurul Shazini Ramlib, Nor Afizah Mustaphaa, and Ismail Fitry Mohammad Rashedia
a
Department of Food Technology, Faculty of Food Science and Technology, Universiti Putra Malaysia, Selangor,
Malaysia; bDepartment of Food Science, Faculty of Food Science and Technology, Universiti Putra Malaysia, Selangor,
Malaysia

ABSTRACT ARTICLE HISTORY


The physicochemical properties, shelf life and stability of pitaya pearls (PP) Received 18 April 2019
by reverse spherification from sodium alginate (PP Alginate), kappa carra- Revised 17 July 2019
geenan (PP Kappa) and a combined iota carrageenan-sodium alginate (PP Accepted 19 July 2019
Iota) were studied. The macronutrients of PP were not affected by the
KEYWORDS
hydrocolloid types, except for ash. PP Alginate showed the strongest tex- Alginate; carrageenan;
tural properties. Storage duration affected mainly elasticity of all PP. During texture; rupture force;
storage, PP Alginate and PP Kappa had better morphological and textural storage stability
stability. However, PP Kappa with lower values of calorie, hardness, and
rupture force is the suggested PP for consumption in beverages.

Abbreviations: ANOVA: Analysis of variance; AOAC: Association of Official


Analytical Chemists; GLM: General Linear Model; PP: Pitaya pearl

Introduction
Tapioca pearls are small spheres (1–6 mm diameter) made from tapioca starch with a shiny surface and
elastic texture.[1] Produced mainly in Thailand, Indonesia and Malaysia, tapioca pearls increase the
calorie in sweet drinks. The total calorie of milk tea containing tapioca pearl served in a small cup
(473 mL) was 299 kcal as compared to milk tea alone (263 kcal).[2] Multiple high-calorie intakes may
contribute to obesity and diabetes.[3] Besides, maleic acid which is a prohibited ingredient in food due to
its toxicity effect[4], is incorporated into tapioca starch to increase the elasticity.[5] Therefore, healthier
pearl ingredients such as pitaya and hydrocolloids are a good alternative to overcome the problems.
Pitaya (Hylocereus polyrhizus) or red dragon fruit originated from Mexico, Central, and South
America.[6,7] It is planted in Thailand, Vietnam, and Malaysia. The fruit is firm, juicy, sweet and has
an intense deep red-purple color caused by an antioxidant called the betalains. Pitaya contains high fiber,
minerals, vitamin C and vitamin A.[8,9] The carbohydrate in pitaya consists of glucose (401 g/kg), fructose
(158 g/kg) and oligosaccharides (89.6 g/kg), where the mixture of oligosaccharides in pitaya stimulates
prebiotic activities.[10] Pitaya also exhibits high antioxidant (betacyanins and betalanins) and antimicro-
bial activities.[11] Pitaya has a fleshy-type texture that is suitable to produce puree or juice, fermented
liquid, and wine.[12] The flesh could be mixed with milk, soft drink, ice cream, jellies, and marmalade.[13]
A few researchers used pitaya as a food ingredient because of its natural red color and good antioxidant
activity.[14–16] Due to its distinct color, taste, nutritional benefit and flavor acceptability, pitaya has the
potential to provide good characteristics as fruit pearl’s core by using reverse spherification method.

CONTACT Radhiah Shukri radhiah@upm.edu.my Department of Food Technology, Universiti Putra Malaysia, 43400 UPM
Serdang, Selangor, Malaysia
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/ljfp.
© 2019 Siti Fatimah Azzahra Bubina, Solihah Mat Alia, Radhiah Shukria, Wan Zunairah Wan Ibadullahb, Nurul Shazini Ramlib, Nor Afizah Mustaphaa
and Ismail Fitry Mohammad Rashedia. Published with license by Taylor & Francis Group, LLC
This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/4.0/),
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
1354 S. F. A. BUBIN ET AL.

Spherification is used to encapsulate ingredients with bad flavor, deliver active compound in drugs
and ingredients in pharmaceuticals, immobilize enzyme and to protect active compound from the
environmental threat.[17] This technique is used to coat liquid material using polymer film by forming
a sphere with a liquid core.[18] Reverse spherification technique provides a better shape of pearl which
requires a mixture of cation and targeted ingredient to be injected into the ionic biopolymer solution.
One of the critical properties of pearl by spherification is to be able to have the sensation of flavor burst
in the mouth when the mouth cavity releases light pressure. The sphere should burst readily and
provide the explosion of flavor or element inside the sphere.[17] The commonly used materials for
spherification technique are edible biopolymers, namely proteins and hydrocolloids.
Alginate, a hydrocolloid, is extracted from brown seaweeds and is a common material used for
material encapsulation, hydrogels, and film gels. It is composed of 1–4 linked α-L-guluronic and β-
D-mannoronic acid residue.[19] Rigid hydrogel beads can be formed by simple gelation with divalent
cation with higher affinity to Ca2+ and result in the egg-box formation.[20] Alginate has broad biological
and food applications due to its biodegradability, biocompatibility, non-toxic and is reasonably
cheap.[21,22] However, alginate hydrogels had poor mechanical properties and porous structure which
are decisive for food or drug delivery system.[22] To enhance the gel properties, sodium alginate is
commonly combined with other polysaccharides, for instance, guar gum, chitosan[23,24] or
carrageenan.[25,26]
Carrageenan is a polysaccharide from certain red seaweed (rhodophyta) species, for instance,
rhodophyceae, furcellariacaea, gigartinaceae, hypnaeceae, phyllophoraseae, and solieriaceae.[27,28]
Kappa and iota carrageenan are commonly used as a gelling agent that have an affinity toward K+
and Ca2+, respectively. Both carrageenans forms a thermoreversible ordered helical structure during
gelation.[29] Kappa and iota carrageenan can form a film in spherification due to its gelling
properties.[30] A film formed from carrageenan and alginate mixture had increased moisture barrier
and tensile properties than alginate alone.[31] Furthermore, the combination of carrageenan and
alginate as polymer microspheres had a lower bursting ability and had increased protection of
internal material in acidic condition.[32] The only study found on the usage of the carrageenan-
alginate mixture in food is the development of encapsulated caffeine.[33] Other studies in carragee-
nan-alginate encapsulation were in the pharmaceuticals field.[25,26,34]
Many researchers have focused on the undesirable health effects of consuming sweetened
beverages containing tapioca pearl.[2,35,36] However, these studies were only limited to characterizing
the nutritional properties and its adverse effects on health, without offering any alternative solutions.
Hence, it is essential to find a healthier alternative for tapioca pearls to improve the nutritional
properties of beverages. In this study, the development of pitaya pearls by reverse spherification by
using carrageenan or combination of alginate-carrageenan are expected to have improved nutri-
tional, morphological and physical properties. The objective of this study was to study the physico-
chemical properties of developed pitaya pearls by using reverse spherification method using alginate,
kappa carrageenan and a combination of alginate-iota carrageenan. The shelf life and stability of
pitaya pearls were also evaluated.

Methods and materials


Materials
Ripe red pitaya fruits were obtained from the local market in Sri Serdang, Selangor. Materials used to
produce the pearls were sodium alginate (R&M), calcium chloride (BisChem), kappa carrageenan
(TA150, Tacara) and iota carrageenan (TS150, Tacara). All chemicals used were food grade.

Preparation of pitaya pearl


Table 1 shows the formulation of pitaya pearls (PP) using different hydrocolloids.
INTERNATIONAL JOURNAL OF FOOD PROPERTIES 1355

Table 1. Formulation of pitaya pearls by using different hydrocolloids.


Pitaya pearls*
Ingredients Alginate Kappa Iota Alginate
Pearl solution
Pitaya puree (g) 500 500 500
Calcium chloride (g) 4 4 4
Bath solution
Distilled water (mL) 100 100 100
Sodium alginate (g) 5 - 2
Kappa carrageenan (g) - 5 -
Iota carrageenan (g) - - 3
* Pitaya pearls produced using bath solutions of sodium alginate, kappa carrageenan
and combination of sodium alginate-iota carrageenan.

Preparation of pitaya puree


Pitaya fruit was peeled and cut into small chunks and fed into juice extractor (MJ-70M Juicer,
Panasonic, Japan) to remove the seeds. The obtained puree was placed in a beaker, heated at 60°C for
30 min in a water bath (ThermoBath, Germany) and cooled in an ice bath. The chilled puree was
then kept in a plastic container and stored at −18°C[37] until further use.

Preparation of pearl solution


Frozen pitaya puree was thawed by leaving it at room temperature (25°C) for 30 min. The puree
(500.0 g) was mixed with calcium chloride (4.0 g) using a hand blender (Tefal HB853866/700–0315-
R, Japan). Then, the pearl solution was transferred into a 250 mL squeezable bottle and left to rest at
room temperature (25°C) for 30 min prior to reverse spherification procedure.

Preparation of bath solution


Three formulations of hydrocolloid (sodium alginate, kappa carrageenan and a combination of iota
carrageenan-sodium alginate) were used to prepare the bath solution as in Table 1. Bath solution was
freshly prepared by mixing 3.0 or 5.0 g hydrocolloid with distilled water (100 mL) using a high-speed hand
blender (Tefal HB853866/700–0315-R, Japan). The amount of hydrocolloid was determined based on
preliminary study (not reported). The mixture was warmed and kept at 75°C for 2 min before transferred
into a beaker.

Preparation of PP by reverse spherification


A 250 mL polypropylene squeezable bottle with a mouth dropper (internal diameter of 0.46 mm)
(Toyogo, Malaysia), was used to extrude droplet by inverting the bottle using retort clamp. The
distance of the mouth dropper to the bath solution surface was 3 cm. The prepared puree solution
was dropped from the bottle into the bath solution and left for 5 min. The PPs formed were collected
and rinsed in distilled water by swirling thrice using a perforated spoon. Then, the pearls were kept
in an airtight container that was then placed in a chiller at 4°C for further analysis and storage study.
Other than storage study, all analyses were carried out on fresh samples.

Chemical analysis and calorie


Determination of protein, fat, ash and moisture were determined based on AOAC Method 990.03,
AOAC Method 920.39., AOAC Method 942.05, and AOAC Method 934.01, respectively. The calorie
content of all the PP was determined according to the equation of the chemical compositions.[38]
1356 S. F. A. BUBIN ET AL.

Physical analysis
Size
The PPs were dabbed with tissue to remove excess water and measured individually by using venire
caliper (Mitutoyo, Japan). The measurement was done in triplicates.

Instrumental texture analysis


One pearl from each formulation was used for the texture profile measurement. Three replicates for
each sample were randomly selected for the tests and placed on a compression plate. A small flat
metal ring was used at the center of the plate to steadily hold the round sample. Samples were tested
for texture profile analysis and burst-ability test using texture analyzer (TPA; Stable Micro Analyzer
TA, XT2i, United Kingdom). A P36R cylinder probe was attached to 5 kg load cell and compression
was set to 75% of its original height with a force of 5.0 g. The pre-test speed, test speed, and post-test
speed was set at 1, 5 and 5 mm/sec, respectively. Properties measured were hardness, cohesiveness,
springiness, and gumminess. The bursting force was determined using the similar parameter as
texture profile analysis except the compression was set at 50% with test speed at 2 mm/sec and post-
test speed at 10 mm/sec. The bursting force was applied to evaluate the rupture force and elasticity.

Colour
Colour analysis was performed on a single pearl for each formulation using a Hunter Lab spectro-
photometer (UltraScan Pro, HunterLab, USA). Three replicates for each sample were randomly selected
for the tests. The mode used was Reflectance Specular Excluded that was specifically for semi-solid
sample with glossy properties. The standard color scale used was CIELAB with parameter L* (lightness/
darkness), a* (+ a = redness, – a = greenness) and b* (+ b = yellowness, – b = blueness).

Storage study
For bursting force (rupture force and elasticity), all samples were collected for 5 (Day 0, 1, 2, 3, 4)
consecutive days at 4 ± 1°C. The duration of storage was determined from a preliminary test (not
reported) which showed that the pearls turned sour at a chilled temperature (4 ± 1°C) on day 5. Each
sample was kept in a round polypropylene container (115 mL) and stored in a larger squared HDPE
container (8 L) under two storage conditions which were chilled (4 ± 1°C) and frozen (−24 ± 5°C).
Samples were thawed to room temperature and tested for rupture force and elasticity. For moisture,
the samples were collected on day 0, 2 and 4; thawed to room temperature (25°C) and tested.

Morphological properties
The PPs at day 0 and 4 were stored at −24°C for 1 day and freeze-dried in a freeze dryer (77550-01H,
Labconco, USA) for 2 days. The morphological properties of PPs at day 0 was observed using
a digital microscope (Eclipse 80i, Nikon, Japan) at 40, 200 and 400 × magnifications. The PPs at day
4 during storage study were observed under a scanning electron microscope (S-3400N Hitachi,
Japan). A single freeze-dried pearl was fixed to a holder and spurred with gold-palladium layer and
viewed at 30 and 300 × magnifications.

Statistical analysis
Except for storage study, all data were analyzed by one-way ANOVA. Storage study data were
analyzed using the general linear model (GLM). GLM on rupture force and moisture were carried
out on 3 × 2 × 5 (formulation, temperature, duration) and 3 × 2 × 3 (formulation, temperature,
duration) factorial designs, respectively. The data were expressed as mean ± standards deviation. The
significant difference between the means of sample attributes was p ≤ 0.05. The means were
expressed in triplicates unless stated otherwise.
INTERNATIONAL JOURNAL OF FOOD PROPERTIES 1357

Results and discussion


Nutritional compositions and calorie of PP
Table 2 showed moisture, protein, fat, and ash of PP. Except for ash, no statistical differences were
observed on all compositions of different hydrocolloids used for the production of PPs. The
insignificant result showed that the nutritional compositions, especially fat were not the contributing
factor to the calorie and the textural properties. Ash in PP Alginate (0.82%) was significantly higher
by two times than PP Kappa (0.35%) and PP Iota (0.31%), indicating higher amounts of minerals.
This is believed to occur due to the extracted alginate from the brown seaweed had higher ash
content than the carrageenan extracted from the red seaweed.[39] However, the result was in
contradictory with Mohammadi et al.[40] where ash was higher in the red seaweed as compared to
the brown seaweed. The difference was probably contributed by separated geographical locations
where Krisnaiah et al.[39] collected seaweeds from the South China Sea, whereas Mohammadi et al.[40]
collected seaweeds from the Northern Persian Gulf. In terms of calorie, PP Kappa had the lowest
(12.86 kcal), followed by PP Iota (15.35 kcal) and PP alginate (17.64 kcal/100 g). The calories were
two times lower than the tapioca pearls (36 kcal) in the study reported by Min et al.[2] proving
a healthier option than the tapioca pearls.

Size and textural properties of PP


Table 3 shows the size and texture profiles of PP. The size of PP Iota was 37% and 33% higher than PP
Alginate and PP Kappa, respectively. When in contact with droplets containing pitaya puree-CaCl2, the
high viscosity of bath solution increased the thickness and stickiness characteristics of PP Iota.
Consequently, the size of PP Iota became bigger. This gelation process improves the cross-linking activity

Table 2. Nutritional compositions and calorie of pitaya pearls.


Pitaya pearls*
Alginate Kappa Iota Alginate
Moisture (%) 94.17 ± 1.66a 95.60 ± 0.15a 95.53 ± 0.02a
Protein (%) 0.17 ± 0.15a 0.26 ± 0.26a 0.17 ± 0.15a
Fat (%) 0.02 ± 0.03a 0.06 ± 0.10a 0.11 ± 0.19a
Ash (%) 0.82 ± 0.37a 0.35 ± 0.03b 0.31 ± 0.09b
Calorie (kcal) 17.64 12.86 15.35
Data are means ± standard deviation. Means within columns not sharing a common letter
are significantly different at p ≤ .05.
* Pitaya pearls produced using bath solutions of sodium alginate, kappa carrageenan and
combination of sodium alginate-iota carrageenan.

Table 3. Size and texture profiles of pitaya pearls.


Pitaya pearls*
Parameter Alginate Kappa Iota Alginate
Size (mm) 4.87 ± 0.23b 5.15 ± 0.09b 7.75 ± 1.22a
Hardness (g) 255.66 ± 16.21a 147.72 ± 13.11b 148.10 ± 6.49b
Cohesiveness 0.41 ± 0.05a 0.27 ± 0.01b 0.28 ± 0.004b
Gumminess (g) 105.91 ± 16.17a 41.51 ± 5.01b 40.86 ± 1.23b
Springiness (mm) 0.39 ± 0.02c 0.79 ± 0.01a 0.47 ± 0.02b
Rupture force (g) 47.62 ± 12.13b 24.22 ± 5.03c 73.11 ± 6.26a
Elasticity (mm) 1.38 ± 0.16a 1.53 ± 0.16a 0.97 ± 0.02b
Data are means ± standard deviation. Means within columns not sharing a common letter are
significantly different at p ≤ .05.
* Pitaya pearls produced using bath solutions of sodium alginate, kappa carrageenan and combina-
tion of sodium alginate-iota carrageenan.
1358 S. F. A. BUBIN ET AL.

PP Alginate PP Kappa PP Iota Alginate

40 × magnification
200 × magnification
400 × magnification

Figure 1. Microstructure of pitaya pearls (PP) at day 0 under a digital microscope at 40, 200 and 400 × magnifications.

with calcium to form a gel.[41] Istini et al.[42] reported the viscosity of kappa was lower (68.17–246 cp) as
compared to iota (147.7–790 cp) that may have produced smaller size of PP.
Desired textural properties of pearls in drinks may vary according to consumer’s preference but
should be soft enough to be burst with optimal chewing sensation. In the study, bursting properties
consist of rupture force and elasticity. PP Alginate had higher hardness, cohesiveness, and gummi-
ness than PP Kappa and PP Iota. However, the springiness of PP Kappa was two times higher than
other samples. In terms of elasticity, PP Iota had a significantly lower value. The low elasticity was
mostly due to thicker gel coating (Figure 1), which will be further discussed in the morphological
structure of PP.
Hardness indicates the stability of the pearl from bursting during processing and storage (Tsai
et al., 2017). The hardness of PP Alginate was 42% higher as compared to PP Kappa and PP Iota.
Hardness was positively correlated with cohesiveness and gumminess since gumminess was a result
of hardness × cohesiveness. PP Alginate had significantly higher cohesiveness and gumminess by 1.5
times and 2.6 times, respectively, than the other two samples. The possible reason was that alginate
gel gave firmer PP encapsulation due to G-block of alginate (alginate oligosaccharide) that per-
formed coordination with calcium ions better than other two hydrocolloids.[17] In comparison, the
hardness of all PP in this study was relatively higher as compared to liquid core hydrogel bead from
alginate produced by Tsai et al.[17], most likely due to the bigger size of all PPs by 10 times.
The springiness of PP Kappa was almost double the value than the other two hydrocolloids. This
result was probably due to kappa carrageenan having a lower affinity to Ca2+ which weakened the
gelation formed. Kappa carrageenan forms a firmer gel in the presence of K+.[43] Rupture force
required to break PP was significantly higher for PP Iota (35% and 68% higher than PP Alginate and
PP Kappa, respectively). In contrast, the elasticity of PP Iota was significantly lower than the other
PP. Low elasticity and high force rupture had explained the resolving texture of the PP Iota after
biting during the preliminary study of sensory evaluation (not reported in the study).
INTERNATIONAL JOURNAL OF FOOD PROPERTIES 1359

Overall, PP Kappa had the best textural properties as compared to the other formulations. The low
hardness, cohesiveness and rupture force with high springiness showed the suitability of PP Kappa to be
burst and chewed at the optimum textural sensations without melting too fast in the mouth or
portraying a chewing gum-like texture. The high hardness, cohesiveness, and gumminess of PP
Alginate may not provide the best textural sensation of PP. Although PP Iota had a few similar textural
properties as PP Kappa, the low elasticity and springiness were not desirable traits of PP. The bursting
properties, moisture content (Table 5) and microstructure (Figure 2) instabilities of PP Iota during four
days of storage further supported the unsuitability of PP Iota Alginate as the gel coating of PP.

Colour of PP
The average color value (L*, a*, b*) characteristics of PPs are given in Table 4. The L* value of PP
was not affected by the different hydrocolloids used for reverse spherification. The a* of PP Kappa
was 1.7–1.8 times lower than PP Alginate and PP Iota. Although b* values of PP Alginate was lesser
and PP Kappa was higher than PP Iota, both were not significantly different from b* value of PP
Iota. These differences in a* and b* indicated the refraction of ultraviolet color during gel formation
due to the pigment present in the red pitaya that contributed to red-purple color, consequently being
responsible for a* and b* chroma.[44]

Storage effect on rupture force, elasticity and moisture content


Table 5 shows the interaction of the main effect of variables (temperature, duration, and formula)
and interacted effect between all the variables for rupture force, elasticity and moisture during
storage by using GLM. Storage duration (main effect) and all variables in the interacted effect gave
an impact to all parameters. Based on all parameters, the optimum conditions during storage were at
4°C (temperature) for 2 days (duration).
The main effect for rupture force was significant for temperature and duration. Lower tempera-
ture and final day of storage had significantly higher rupture force. The temperature at −24°C and
longer storage duration may have caused moisture leaching that caused shrinkage of PP, conse-
quently increasing the rupture force. There was a significant interaction effect observed between
hydrocolloid formula and duration as well as interactions between all variables with R2 of 68.08%.
The elasticity of pearls was all affected by main effect and each of their interacted effects. The
elasticity of all PP stored at −24°C significantly reduced as compared to 4°C condition, most likely
due to water expulsion from the gel at a lower temperature. The main effect of the formula was in
agreement with the elasticity measurement (Table 3) where PP Alginate had the highest value,
followed by PP Kappa and PP Iota. In addition, the longer duration of storage caused higher
elasticity. This result can be explained by possible cross-linking of gel during storage that enhanced
the hydrocolloid’s molecular interaction, consequently increasing the elasticity. The R2 of elasticity
for all interaction effect for all variables was 82.30%, which indicated a well-fitted model.
Moisture content was only being affected by storage duration where a significant decrease was
observed on day 4. This result was expected because moisture loss occurrence is common during storage
that may have affected the other variables. Although insignificant, the moisture content of PP Iota was
lower than other PP formula. For moisture, all variables had interacted effects with R2 of 58.02%.

Morphology structure of PP
The digital microscope photos of PPs on day 0 are presented in Figure 1 and morphology of PPs
after 4 days of storage by SEM is presented in Figure 2. Generally, PP Alginate had the smoothest
surface morphology, followed by PP Kappa and PP Iota. PP Alginate had dense and fine lines that
indicated small folds. However, the surface was smooth, consistent and showed a homogenous
thickness probably due to sturdy gelation. This factor contributed to the high hardness, cohesiveness,
1360

PP Alginate PP Kappa PP Iota Alginate


S. F. A. BUBIN ET AL.

30 × magnification
300 × magnification
Figure 2. Microstructure of pitaya pearls (PP) after 4-days storage at −24°C observed under a scanning electron microscope at 30 and 300 × magnifications.
INTERNATIONAL JOURNAL OF FOOD PROPERTIES 1361

Table 4. Colour attributes of pitaya pearls.


Pitaya pearls#
Alginate Kappa Iota Alginate
L* (Lightness) 19.97 ± 1.44a 18.30 ± 0.21a 18.71 ± 0.39a
a* (Redness) 15.84 ± 0.80a 8.69 ± 0.31b 14.70 ± 0.90a
b* (Blueness) −3.28 ± 0.43a −4.40 ± 0.30b −3.85 ± 0.24ab
Data are means ± standard deviation. Means within columns not sharing a common letter are
significantly different at p ≤ .05.
#
Pitaya pearls produced using bath solutions of sodium alginate, kappa carrageenan and
combination of sodium alginate-iota carrageenan.

gumminess, and elasticity (Table 3). The good elasticity and moisture retention during storage were
also reflected by its maintained smooth surface and minimal shrinkage at day four (Figure 2). This
result is supported by Xu et al.[45] where a membrane film developed from alginate showed a lower
degree of roughness.
At day 0, PP Iota appeared thicker, less smooth and had more folds and wrinkles than PP
Alginate (Figure 1). The structure probably resulted from the interaction of sodium alginate and iota
carrageenan that formed a gel with higher cross-linking, consequently increasing the folds and
unevenness. When the membrane was replaced with an increased amount of carrageenan, holes
appeared on the surface[45], which was more evident after 4 days of storage (Figure 2). PP Iota had
a more intense red color with a thicker gel coating. The thicker coating may be the cause of
significantly higher rupture force and lower elasticity (Table 3). After storage, PP Iota had
a rougher surface, cracks and was porous (Figure 2), which correlates with the low retention of
moisture content during storage (Table 5). The heterogeneous structure of PP Iota may cause
brittleness, which probably was caused by the expulsion of water during storage at frozen
temperature.[45] This structural surface was related to the severe loss of moisture after storage at
−24°C for 4 days as discussed in the interaction of all variables for moisture content during storage.
PP Kappa at day 0 had more folds and thinner structure than the other PPs (Figure 1), which may
explain the significantly lower rupture force (Table 3). PP Kappa also had a lighter red color, but
appeared to be more blue purplish in hue than other PP’s, which was in proportion with its a* and b*
values (Table 4). The blue hue was more evident probably due to the thinner membrane of PP
Kappa. Although PP Kappa appeared less uniform than PP Alginate after storage (Figure 2), the
morphological structure appeared consistently homogenous in terms of smoothness and was not as
degraded as PP Iota.

Conclusion
Except for ash, different hydrocolloids used in the formulation did not affect the macro nutritional
composition of PPs. However, PP Kappa showed the best performance in the textural properties with
intermediate values which was suitable for optimum textural sensation in mouth, which can be
confirmed in sensory test as a future analysis. PP Kappa also had lower calorie, optimum elasticity
and acceptable morphological structure stability in the storage study. Storage study showed that
interacted effect of variables (formula, duration, and temperature) prominently affected elasticity
compared to rupture force and moisture of PPs. For better textural properties, it is suggested that
PPs produced from reverse spherification method is best to be stored up to 2 days at 4°C. Further
studies on the stability of pitaya’s antioxidant and nutritional properties during storage should be
considered. Additionally, stability of PPs in different beverage temperatures and its effect on the
viscosity of beverages should be studied too. PPs formed by reverse spherification method was able
to encapsulate the pitaya puree and has the potential of replacing the unhealthy tapioca pearls. The
study showed a promising potential of kappa carrageenan as pearls gelling agent for pitaya puree
filling in dessert and beverage industries.
1362
S. F. A. BUBIN ET AL.

Table 5. Storage variables (temperature, duration, and formula) effect on rupture force, elasticity and moisture content of pitaya pearls.
Main effect Interacted effect
Temperature Formula & Formula & Temperature & Formula & Duration &
Parameters (°C) Duration (day) Formula# Temperature Duration Duration Temperature
4 −24 0 1 2 3 4 A K IA
Rupture force
Mean (g) 38.25 52.12 46.17 48.27 34.42 40.36 56.69 49.45 43.51 42.58
P-value 0.00 0.00 0.20 0.31 0.00 0.12 0.00
R-squared 68.08
Elasticity
Mean (mm) 1.37 1.08 1.19 1.37 1.08 1.10 1.39 1.40 1.27 1.01
P-value 0.00 0.00 0.00 0.00 0.00 0.00 0.00
R-squared 82.30
Moisture
Mean (%) 91.59 90.65 94.16 - 92.17 - 87.04 91.52 92.10 89.75
P-value 0.42 0.00 0.24 0.11 0.69 0.98 0.03
R-squared 58.02
The main effect and interacted effect variables are significantly different when p-value is <.05.
#
Pitaya pearls produced using bath solutions of sodium alginate (A), kappa carrageenan (K) and combination of sodium alginate and iota carrageenan (IA).
INTERNATIONAL JOURNAL OF FOOD PROPERTIES 1363

Acknowledgments
We thank the Faculty of Food Science and Technology and Institute of Bioscience, both located in Universiti Putra
Malaysia for funding and usage of equipment.

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