ARTICLE IN PRESS

FOOD
HYDROCOLLOIDS
Food Hydrocolloids 21 (2007) 928–935
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Characteristics of microencapsulated b-carotene formed by spray drying

with modified tapioca starch, native tapioca starch and maltodextrin
Jarunee Loksuwan
Department of Food Science and Technology, Faculty of Science and Technology, Thammasat University, Pathumthani 12120, Thailand
Received 14 June 2006; accepted 25 October 2006

Abstract

Acid-modified tapioca starch, native tapioca starch, and maltodextrin were tested for their ability to serve as wall materials for
encapsulating b-carotene. The modified tapioca starch had wider particle size distribution, toward the smaller diameters, as compared to
its native starch and maltodextrin. Moisture content and water activity of microcapsules were found to be dependent on type of wall
materials. There were differences in total b-carotene and surface b-carotene contents among samples. The total b-carotene was highest
for modified tapioca starch while it was lowest for maltodextrin. The surface b-carotene was lowest for modified tapioca starch while it
was highest for native tapioca starch. The modified tapioca starch was more effective than its native starch in b-carotene retention.
Results obtained suggest that the modified tapioca starch can be considered as potential wall material for encapsulation of b-carotene.
r 2006 Elsevier Ltd. All rights reserved.

Keywords: Tapioca starch; Microencapsulation; b-carotene; Spray drying; Steam pressure

1. Introduction form a stable emulsion. The emulsion is then fed into a

Microencapsulation is the technique by which the
sensitive ingredients are packed within a coating or wall
material. The wall material protects the sensitive ingredient
(or core) against adverse reaction, prevents the loss of
volatile ingredient, and controls release of the ingredient
(Risch, 1993; Shahidi & Han, 1993). In addition, micro-
encapsulation can convert liquids into free-flowing powers,
which are easy to handle.
Microencapsulation has found many applications in
food industry. Important applications are to coat color-
ants, flavors, vitamins, and other sensitive food ingredients
in order to increase their shelf life (Dziezak, 1988; Shahidi
& Han, 1993). Various techniques are employed to
microencapsulate food ingredients. Spray-drying is the
most often used technique in the food industry (Gibbs,
Kermasha, Alli, & Mulligan, 1999; Reineccius, 1988). In
this process, the sensitive ingredient was mixed or
homogenized in a solution containing wall material to
Tel./fax: +66 2 564 4486.
E-mail address: jarunee@alpha.tu.ac.th.
spray dryer where it is converted to a dried particle.
Numerous wall materials or encapsulating agents are
available for food application. Gums arabic, hydrolyzed
starches, and emulsifying starches are most commonly used
as wall materials (Kenyon, 1995; Reineccius, 1988; Shahidi
& Han, 1993). Some proteins such as whey proteins
(Sheu & Rosenberge, 1995), sodium caseinate (Hogan,
McNamee, Riordan, & Sullivan, 2001), and gelatin
(Bruschi, Cardoso, Lucchesi, & Gremiao, 2003) are also
used as wall materials. Typically, the effective wall
materials for spray drying should have functional proper-
ties, including good emulsification, film forming, high
solubility, low viscosity at high concentrations and low cost
properties (Reineccius, 1988; Trubiani & Lacourse, 1988).
Gum arabic, a natural plant exudates polysaccharide of
acacia, is a well-known effective wall material for many
years and is still the good choice as wall material due to its
stable emulsion and good volatile retention. Problems
associated with the use of gum arabic in microencapsula-
tion are high cost and limited supply. Emulsifying
starches are starches derivatives with lipophilic group, i.e.
1-octenyl succinate. These wall materials have excellent

0268-005X/$ - see front matter r 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.foodhyd.2006.10.011
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J. Loksuwan / Food Hydrocolloids 21 (2007) 928–935
emulsification properties (Trubiani & Lacourse, 1988).
However, emulsifying starches have some limitations. They
exhibit poor flavor protection against oxidation and have
off flavor (Reineccius, 1988). Krishnan, Kshrisagar, and
Singhal (2003) studied the efficacy of succinylated waxy
maize starch, maltodextrin and gum arabic as wall
materials for encapsulation of cardamom oleoresin by
spray drying. They reported that succinylated waxy maize
starch and maltodextrin had a lower protection to
cardamom oleoresin during storage as compared to gum
arabic. Maltodextrins are hydrolyzed starches produced by
partially hydrolysis of starch with acid or enzymes.
Hydrolyzed starches have the advantages of being low
cost, bland in flavor, and good flavor protection against
oxidation. Hydrolyzed starches are reported to improve
shelf life of orange oil (Anandaraman & Reineccius, 1986)
and carrot carotene (Wagner & Warthesen, 1995). These
authors also reported that storage stability of core
materials increased as hydrolyzed starches DE increased.
Problems associate with the use of hydrolyzed starches in
microencapsulation are lack of emulsification properties
and poor flavor retention (Reineccius, 1988). Many
researches have used hydrolyzed starches in conjunction
with other wall materials or emulsifying agents to improve
their emulsifying characteristics. Mixtures of maltodextrins
or corn syrup solids with whey proteins were reported as
effective wall materials for microencapsulation of ethyl
caprylate (Sheu & Rosenberge, 1995). Barbosa, Borsarelli,
and Mercadante (2005) reported that maltodextrin with
emulsifier Tween 80 had the ability to encapsulate a higher
amount of bixin than maltodextrin alone. A blend of gum
arabic: maltodextrins: modified starch at a 4/6:1/6:1/6
was reported to provide a better protection of cardamom
oleoresin than gum arabic (Krishnan, Bhosale, & Singhal,
2005).
Preliminary study in our laboratory has shown that the
efficacy of acid modified starch for encapsulation required
the starch pre-swelling and gelatinization. This can be
achieved by autoclaving of the modified starch slurry under
steam pressure. This process results in formation of starch
paste. The objective of this study was to evaluate the
potential of acid modified tapioca starch after treated with
heat under steam pressure as wall materials for encapsula-
tion of b-carotene. The microstructure and physicochem-
ical properties of encapsulated powder were investigated.
These results were compared to those of its native starch
and commercial maltodextrin.
2. Material and methods
2.1. Materials
Native tapioca starch was purchased from local market
(Thailand). The moisture content was about 8%.
Moisture content was determined according to the method
described in Section 2.9. Maltodextrin (Star-Dri 240-S, DE
24) was a gift from Burley Jucker Specialties Ltd.
929
(Bangkok, Thailand). Modified tapioca starch was
prepared according to the method described in
Section 2.2 in the laboratory of Department of Food
Science and Technology of Thammasat University
(Pathumthani, Thailand). Trans-b-carotene (powder) was
obtained from Sigma Chemical Company (St. Louis,
USA). All other chemicals used in this study were of
analytical grade.
2.2. Sample preparation
Acid modified tapioca starch was prepared from
native tapioca starch according to the procedure of
Loksuwan (2005) (Thailand Petty Patent No. 2146).
Tapioca starch was added to 3 N H2SO4 in a ratio of
1:5 w/v. The mixture was stirred magnetically for 3 h at
60 1C. After hydrolysis the starch slurry was cooled and
neutralized with saturated Na2CO3. The acid modified
starch was filtered, washed with three volumes of distilled
water, followed with 100 ml ethanol (95%). The starch
was then dried at 70 1C for overnight. The dried starch
was ground using a laboratory blender. Prior to micro-
encapsulation, the modified starch was suspended in
distilled water (29% w/w) and heated under steam pressure
for 5 min to obtain gelatinized starch paste. Pure trans-
b-carotene was added to the gelatinized starch paste in a
ratio of 1:580 w/w, on dry starch basis. The mixture was
then homogenized to obtain an aqueous emulsion
(feed liquid) and immediately fed to the spray-dryer
(Armfield FT 30, Armfield Technical Education Co.,
Hampsshier, England). The inlet and outlet air tempera-
ture were maintained at 17075 and 9575 1C, respectively.
Experiments were performed in triplicate. The spray-dried
powders were collected, kept in plastic bags wrapped with
aluminum foil and stored in desiccators containing silica
gel at room temperature.
Solution of maltodextrin (29% w/w) and native tapioca
starch (20% w/w, due to limit of viscosity) in distilled water
were used for comparison study. Pure trans-b-carotene was
added to maltodextrin and native tapioca starch solutions
in the ratio of 1:580 and 1:400 w/w, on dry basis,
respectively. The homogenization and spray drying were
performed in the similar manner above.
2.3. Determination of dextrose equivalent (DE) and
viscosity
DE of modified starch produced by acid hydrolysis was
determined using the method of Lane and Eynon (1923).
Viscosity (cps) of samples was measured using Brook-
field Digital Viscometer (Model DV-II+, Brookfield
Engineering Laboratories, Inc., Stoughton, USA). Solu-
tions of modified tapioca starch (29% w/w), native starch
(20% w/w), and maltodextrin (29% w/w) in distilled water
were prepared. The samples were then placed in a water
bath with gently stirred. The viscosity was measured when
the temperature of sample reached 80 1C.
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930 J. Loksuwan / Food Hydrocolloids 21 (2007) 928–935
2.4. Particle size distribution
The particle size distributions of the spray dried powders
were determined using Laboratory test sieve (AS 200 digit,
ASTME 11, Retsch, Germany).
2.5. Optical microscope
An optical microscope (Polarizing Microscope Axios-
kop-po, Zeiss) was used to investigate the feed liquids
before spray drying and the spray dried powders. The
picture was taken at 200  magnification.
2.6. Scanning electron microscopy
Scanning electron microscope (SEM) (JEOL JSM-6301F,
Jeol Ltd., Tokyo, Japan) was used to study the morpholo-
gical properties of the spray-dried powders. Powder particles
were attached to the SEM stubs of 100 diameter using a two-
sided adhesive tape. The samples were then sputter coated
with gold and examined at 500  , 1000  , and 1500 
magnifications. An acceleration potential of 5 kV was used
during micrograph.
2.7. Analysis of total and surface carotene of spray-dried
powder
The method of Desobry, Netto, and Labuza (1997) with
slight modification was used to analyze the total carotene
and surface carotene.
Total carotene: Powder (50 mg) was weighed into the
125 ml-flask, dispersed in water (2.5 ml) and extracted with
hexane (25 ml). After shaking (500 rpm) for 30 min at room
temperature, the hexane fraction was measured at 454 nm
with spectrophotometer.
Surface carotene: Powder (50 mg) was weighed into the
flask and extracted with 25 ml hexane. After shaking at
100 rpm for 15 s, sample was centrifuged at 1000g for
1 min. The supernatant was measured at 454 nm with
spectrophotometer.
2.8. Cold water solubility of spray-dried powders
The method of Singh and Singh (2003) with slight
modification was used to analyze cold water solubility of
spray dried powders. One gram of powder was mixed with
100 ml of water using a magnetic stirrer at room temperature
for 30 min. A 30-ml aliquot of starch solution was transferred
to a 50-ml centrifuge tube and centrifuged (Hettich
Zentrifugal Universal 16R, German) at speed 430g for
15 min. A 10-ml aliquot of the supernatant was evaporated
on a steam bath and dried in an oven at 110 1C for overnight.
2.9. Determination of moisture content and water activity
The moisture content of the samples was measured
by hot air oven at 105 1C for 16 h. The water activity
of the samples was measured using an AquaLab
(CS2, USA).
2.10. Statistical analysis
The data reported in all tables are average of triplicate
determinations. Analysis of the data was carried out using
ANOVA (SPSS program version 10.0 for Windows).
Differences between means were tested using the Duncan’s
multiple range tests at Po0.05.
3. Results and discussion
3.1. Dextrose equivalent (DE) and viscosity
DE is a measure of degree of hydrolysis of starch
molecule, which related to reducing sugar production. The
low DE value means lower amount of reducing sugar
produced. The modified starch obtained in this investiga-
tion had DE value of 2, indicating that degree of hydrolysis
was very low. This means that the acid-modified starch
obtained in this investigation contained less amount of low
molecular weight sugar than maltodextrin with DE value
of 24. In other words, this modified starch contained many
amylose molecules with shorter chain length, as the result
of acid hydrolysis.
Results from the measurement of viscosity showed that
at 29% w/w maltodextrin had lower viscosity (13.8 cps)
than modified tapioca starch (133.8 cps). At 29% the native
starch solution was too viscous to measure its viscosity.
Therefore, the viscosity of native starch was measured at
20% w/w, which was found to be 31,880 cps.
3.2. Particle size distribution
The particle size distributions of spray-dried powders or
microcapsules using Laboratory test sieve are shown in
Fig. 1. The weight percent data were plotted against the
particle diameter in microns. Modified tapioca starch had
wider particle size distribution, toward the smaller
diameters, as compared to its native starch and maltodex-
trin. The most predominant diameters for modified tapioca
starch were 75–150 m (55.8%), for native starch were
106–250 m (69.7%) and for maltodextrin were 106–250 m
(80.0%). The larger powder particle sizes of maltodextrin
can be explained by agglomeration or caking of powder
particles, which were observed in this sample.
3.3. Optical microscope
Light micrographs of feed liquids and spray-dried
powder are showed in Figs. 2 and 3, respectively. Results
clearly showed significant differences among wall materi-
als. The modified tapioca starch showed disintegration of
some granules; only a few starch granules still exhibited
maltese cross as compared with the native starch. This
result indicated that steam pressure treatment caused
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a 60
50
Weight (%)

40
30
20
10
0
< 75 75-106 106-150 150-250 250-300 300-500 500-850 > 850
Particle diameter (u)

b 60
50
Weight (%)

40
30
20
10
0
< 75 75-106 106-150 150-250 250-300 300-500 500-850 > 850
Particle diameter (u)
c
60
50
Weight (%)

40
30
20
10
0
< 75 75-106 106-150 150-250 250-300 300-500 500-850 > 850
Particle diameter (u)
Fig. 1. Particle size distribution of spray-dried powders of b-carotene in
(a) modified tapioca starch, (b) native tapioca starch, and (c) maltodextrin.

changes in granular structure of acid modified starch. In

the case of maltodextrin, completely disintegration of
starch granules was observed.

3.4. SEM of spray-dried powders

Spray-dried powders prepared from modified tapioca

starch, native tapioca starch, and maltodextrin were
observed for granular structure using SEM (Figs. 4
and 5). Results clearly showed significant differences in
size and shape. Microcapsules from modified tapioca
starch showed spherical shape with extensive dented
surface, while those from native tapioca starch showed
rounded shape, smooth surface with no obvious dents.
Modified tapioca starch had granules size ranging from o5
to 30 mm, while native tapioca starch had more homo-
geneous granules ranging in size from 2 to 18 mm.
Formation of dented surfaces of spray-dried particles was
attributed to the shrinkage of the particles during the
Fig. 2. Light micrographs of in feed liquid. (a) Modified tapioca starch,
(b) native tapioca starch and (c) Maltodextrin.
drying process (Rosenberg, Kopelman, & Talmon, 1985,
1990). The extensive dented surfaces of modified tapioca
starch was probably attributed to starch granule disrupted
resulted in more susceptible to shrinkage during the drying
stages. The SEM micrograph of spray-dried maltodextrin
showed spherical shapes with smooth and some dented
surfaces, and a more heterogeneous size, which mainly
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932 J. Loksuwan / Food Hydrocolloids 21 (2007) 928–935
Fig. 3. Light micrographs of spray dried powders of b-carotene in
(a) modified tapioca starch, (b) native tapioca starch and (c) maltodextrin.
consisted of very small granules size o7 mm and few large
size of 7–17 mm. The less dented surface of maltodextrin
comparing to modified tapioca starch could be attributed
to the difference in sugar composition. Maltodextrin used
in this study had DE of 24. Therefore, it consisted of a
greater amount of low molecular weight sugar. These low
molecular weight sugars may act as a plasticizer preventing
shrinkage of the surface during drying. According to
Fig. 4. SME (500  ) of spray dried powders of b-carotene in (a) modified,
tapioca starch, (b) native tapioca starch, and (c) maltodextrin.
Zhang, Ping, and Xiao (2000) plasticizer is important for
the formation of spherical microcapsules with smooth-
surface. Bruschi et al. (2003) used gelatin to encapsulate
propolis by spray drying and reported that addition of
mannitol to gelatin resulted in smooth-surfaced micro-
particles of propolis.
3.5. Cold water solubility of spray-dried powders
Cold water solubility among spray-dried powders showed
significant (Po0.05) differences (Table 1). Modified tapioca
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J. Loksuwan / Food Hydrocolloids 21 (2007) 928–935
Fig. 5. SME (1500  ) of spray-dried powders of b-carotene in
(a) modified tapioca starch, (b) native tapioca starch, and (c) maltodextrin.
Table 1
Cold-water solubility of spray-dried powders of b-carotene in (A)
modified tapioca starch, (B) native tapioca starch, and (C) maltodextrin
Type Cold water solubility
A 90.2572.21b
B 2.2770.39a
C 98.4370.28c
Mean of three replicates; means within column followed by different
superscripts, are significantly different at Po0.05 by Duncan’s test.
933
Table 2
Moisture content and water activity of spray dried powders of b-carotene
in (A) modified tapioca starch, (B) native tapioca starch, and (C)
maltodextrin
Type Moisture content (%) Water activity
A 3.1270.39b 0.2970.09ab
B 6.0070.62c 0.3770.04b
C 2.1170.47a 0.2270.02a
Mean of three replicates; means within column followed by different
superscripts, are significantly different at Po0.05 by Duncan’s test.
starch had higher cold-water solubility than its native starch.
Maltodextrin had the highest cold-water solubility, com-
pletely soluble. These differences could be attributed to the
differences in granular structure. Treatment of tapioca
starch with acid resulted in partial depolymerization of
starch into smaller molecules resulted in a greater amount of
more soluble components. When this starch was heated
under steam pressure, the tight organization of starch
granules was disrupted, which facilitated the migration of
water into the granules and additional leaching out of
soluble components. This resulted in an increase in solubility
of modified starch.
3.6. Moisture content and water activity of spray-dried
powders
Moisture contents and water activity of spray-dried
powders are shown in Table 2. Moisture contents of spray-
dried powders varied from 2.11–6.00% and were differed
significantly (Po0.05). Modified tapioca starch showed
lower moisture content than its native starch. Maltodextrin
had the lowest moisture content. Similar results were
observed for water activity. These differences could be
attributed to the structure of granules and viscosity of
starch. Native tapioca starch had more rigid or tight
crystalline structure and high viscosity (as mentioned
earlier), as compared to modified tapioca starch and these
could influence rate of drying.
3.7. Total carotene and surface carotene of spray-dried
powders
Total carotene and surface carotene contents among the
powders are shown in Table 3. There were significant
differences in total carotene and surface carotene contents
among the wall materials used. Modified tapioca starch
had higher total carotene content (82.18%) than its native
starch (68.35%). Maltodextrin showed the lowest total
carotene content (46.74%). Surface carotene contents of
the dried powders ranged from 19.59% to 104.08%.
Modified tapioca starch had the lowest surface carotene
while native tapioca starch had the highest surface
carotene. These results indicated that, of the wall material
studied, modified tapioca starch treated with steam
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934 J. Loksuwan / Food Hydrocolloids 21 (2007) 928–935
Table 3
Total carotene and surface carotene contents of spray dried powders of b-
carotene in (A) modified tapioca starch, (B) native tapioca starch, and (C)
maltodextrin
Type Total carotene (%) Surface carotene (%)
A 82.1871.47b 19.5971.40a
B 68.3573.76c 104.0873.66c
C 46.7476.56a 73.0274.37b
Mean of three replicates; means within column followed by different
superscripts, are significantly different at Po0.05 by Duncan’s test.
pressure had the highest encapsulation efficiency. This was
probably due to the composition of modified tapioca starch
after steam pressure treatment. The free soluble amylose
associated to form a continuous network joint by hydrogen
bonds, resulting in a gel structure that entrapped b-
carotene in this structure. In addition, amylose is good in
film forming ability; therefore, the presence of high levels of
free soluble amylose of modified tapioca starch may have
advantages of a rapid crust forming around the b-carotene
preventing the loss of b-carotene during drying process.
Major lost of volatiles during spray drying was reported to
occur at the very early stages of drying process (Reineccius,
1988). Therefore, wall materials, which can form film
rapidly at the surface of drying droplet will exhibit a better
flavor retention during drying. Rosenberg et al. (1990)
reported that increase of soluble solids concentration
resulted in decreased the time required for powder crust
formation, and consequently, losses of volatiles were
reduced. In the case of maltodextrin, the low total carotene
content obtained was probably due to the lack of
emulsification and low film-forming capacity resulted in
poor b-carotene retention during drying. Maltodextrin
used in this study contained molecules, which are too small
to impart the emulsifying characteristics. The high-surface
carotene content observed for native tapioca starch could
be attributed to the high viscosity of the starch. High
viscosity caused an increase in time of droplet formation
and internal mixing (Rosenberg et al., 1990). And these
may allow the carotene to migrate to the surface prior to
the formation of dry crust around the particles.
4. Conclusion
The results of this study indicate laboratory prepared
acid modified tapioca starch after treated with steam
pressure has the potential for use as wall material. Acid
treatment in combination with steam pressure yields starch
with low viscosity at high solid. This starch provided good
retension of b-carotene during drying process. The
low-surface carotene contents were also observed for this
modified tapioca starch which indicates better microen-
capsulation efficiencies. Spray-dried powders from
modified tapioca starch showed higher cold-water solubi-
lity than its native starch. Changes in surface morphology
were observed for microcapsules obtained from laboratory
prepared acid modified tapioca starch as compared to its
native starch.
Acknowledgments
This study was financially supported by National
Research Council of Thailand. The author would like to
thank Burley Jucker Specialties Ltd. (Bangkok, Thailand)
for providing maltodextrin.
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