Journal of Food Engineering 104 (2011) 36–42

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Journal of Food Engineering

journal homepage: www.elsevier.com/locate/jfoodeng

Physical characterization of rice starch spherical aggregates produced

by spray-drying
Sara Beirão-da-Costa a,b,c,⇑, Cláudia Duarte a, Margarida Moldão-Martins a, M. Luísa Beirão-da-Costa a
a
CEER – Biosystems Engineering, Instituto Superior de Agronomia, Technical University of Lisbon, Tapada da Ajuda, 1349-017 Lisboa, Portugal
b
IBB – Institute for Biotechnology and Bioengineering, Centre of Biological Engineering, University of Minho, Campus de Gualtar, 4710-057 Braga, Portugal
c
Chemistry Department – Research Unit QOPNA – University of Aveiro, Campo de Santiago, 3810-193 Aveiro, Portugal

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

Article history: The effect of solids content and the presence of bonding agents (CMC and/or gelatin) on the physical char-
Received 22 September 2010 acteristics of rice starch spherical aggregates were investigated. Rice starch spherules were produced by
Received in revised form 23 November 2010 spray-drying at 120 °C according to a 2(k  p) Fractional Factorial Designs at 2 Levels. Particle size analysis,
Accepted 28 November 2010
spherules’ morphology, porosity and crystallinity determination were obtained for the aggregates pro-
Available online 9 December 2010
duced. Results showed that the size of spherules is significantly affected by starch concentration while
the presence of bonding agents seems not to have a direct influence in particle size. The drying process
Keywords:
did not yield a change in crystal type but the presence of gelatin leads to a decrease in crystalline regions.
Starch
Spherules
Starch and bonding agents’ concentrations did not significantly affect neither the total porosity of the
Morphology samples nor the average pore diameter. Intra-particle porosity is mainly dependent on starch and gelatin
Porosity concentrations. This study would be helpful in establishing the more adequate conditions useful in an
Spray-drying industrial application on encapsulating bioactive compounds.
Ó 2010 Elsevier Ltd. All rights reserved.

1. Introduction
Microencapsulation is a technology that allows sensitive
ingredients to be physically entrapped in a homogeneous or heter-
ogeneous matrix aiming their protection. The development of
encapsulation delivery systems (‘‘wall’’ materials) that carry, pro-
tect, and deliver functional food ingredients (‘‘core’’ materials) to
their specific site of action are one of the present challenges in food
engineering.
Spray-drying is a unit operation by which a liquid product is
atomized in a hot gas current to instantaneously yield a powder.
The initial feed material can be a solution, an emulsion or a suspen-
sion and the final product obtained, depending also on operating
conditions, can be a powder with particles in the range of 10–
50 lm (Gharsallaoui et al., 2007).
The choice of the wall material is an important step for the suc-
cess of the microencapsulation process. Traditionally this selection
involved trial-and-error procedures in which the microcapsules are
formed and then evaluated for encapsulation efficiency and stabil-
ity (Pérez-Alonso et al., 2003).
Acacia gum, commonly called gum arabic, was the encapsulat-
ing agent of choice for many years due to its excellent emulsifica-
⇑ Corresponding author at: CEER – Biosystems Engineering, Instituto Superior de
Agronomia, Technical University of Lisbon, Tapada da Ajuda, 1349-017 Lisboa,
Portugal. Tel.: +351 21 3653246; fax: +351 21 3653200.
E-mail address: sarabeirao@isa.utl.pt (S. Beirão-da-Costa).
tion properties but supply shortages and high cost have forced to
look for substitutes (Dickinson, 2003). It was used to encapsulate
several compounds namely volatile aroma compound (Brückner
et al., 2007) and cumin oleoresin (Kanakdande et al., 2007). A wide
variety of natural and synthetic polymers had been used as wall
materials, the selection being dependent, upon other factors, on
the core material (Gharsallaoui et al., 2007).
Among others, the most popular polymers for food ingredient
encapsulation include gelatin (Shu et al., 2006; Chiu et al., 2007),
modified starches (Brückner et al., 2007; Kanakdande et al.,
2007) and whey protein (Brückner et al., 2007).
Carbohydrates such as starches, corn syrup solids and malto-
dextrins have been considered as good encapsulating agents be-
cause they exhibit low viscosities at high solids content and good
solubility (Gharsallaoui et al., 2007).
Zhao and Whistler (1994) observed the ability of small granules
size starch, such as amaranth starch, small granule wheat starch
and rice starch, to form porous spherical aggregates with potential
to encapsulation. The aggregates resemble popcorn balls that can
carry food ingredients within the open spaces of the porous struc-
ture. These spheres are produced when starch suspensions are sub-
jected to spray-drying in the presence of bonding agents, like
polysaccharides or proteins, and any temperature that does not
gelatinize starch appears to be acceptable. The encapsulation
process suggested was the immersion of these structures in the
core material followed by a filtration process. Later on other works
refer the success of these structures in entrapment of ascorbic acid

0260-8774/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2010.11.024
 S. Beirão-da-Costa et al. / Journal of Food Engineering 104 (2011) 36–42
Fig. 1. Schematic representation of porous geometry. Ink-bottle or blind pores (A); cylindrical open-ended pores (B); cylindrical open-ended cross-linked pores(C); closed
pores (D). (Adapted from: Giesche, 2006).
(Trindade and Grosso, 2000) and vanillin (Tari and Singhal, 2002;
Tari et al., 2003). These authors concluded that the incorporation
of the core in the wall material prior to the drying step is also effec-
tive for the encapsulation procedure.
However, the influence of parameters such as concentration of
starch and of bonding agents’, and the end result on physical char-
acteristics of the formed spherical aggregates, namely on the avail-
able void volume for encapsulation, are not known. The knowledge
on these characteristics is important and useful to understand and
predict the encapsulation mechanism and the stability of the en-
trapped compound(s). The pore volume of the porous structure
will probably be limitative of core material retention capacity
but pore size distribution may also affect the degree of protection
offered by spherical aggregates. Additionally, the geometry of
formed pores may influence the subsequent delivery of the en-
trapped compound in the food system (Fig. 1).
The closed pores (D type), obviously will not be available for the
encapsulation process, as the core material has no way of entering.
Only the open pores’ network within the particle can be functional
for retention of active ingredients but the different types of geom-
etry will influence the effectiveness and the rate of their release.
Ink bottle pores (A), despite the volume available to support core
material will offer a higher resistance, comparing to open-ended
ones, to the diffusion of encapsulates due to the difference in
throat and cavity diameters.
The objective of the present work is to better understand rice
starch spherical aggregates production by spray-drying, depending
on starch and bonding agents’ concentration and the physical char-
acterization of the formed aggregates, in terms of particle size dis-
tribution, crystalline structure and porous structure, in order to
predict the more adequate conditions useful for an industrial appli-
cation on encapsulating bioactive compounds.
2. Materials and methods
2.1. Materials
A commercial source of rice starch (10.6 ± 0.78% humidity;
0.6 ± 0.13% protein; 0.06 ± 0.008% total fat; 28.0 ± 0.35% amylose)
was obtained from Remy Industries (Belgium). Carboxymethylcel-
lulose (CMC) and gelatine (80–100 blooms) were obtained, respec-
tively, from Fluka (Sweden) and PANREAC (Spain). Isopropyl
alcohol was purchased from Riedel-de-Haën.
2.2. Methods
2.2.1. Preparation of spherical aggregates
Rice starch was dispersed in water at room temperature (about
22 °C) and the mixture homogenized thoroughly for 30 min with
magnetic stirring. The addition of different binding agents (CMC
and gelatin) was tested. When binding agents were added, those
were previously dissolved in water at 40 °C.
Spherical aggregates were produced by spray drying of rice
starch suspensions in a LabPlant SD-04 (Leeds, UK) spray dryer
equipped with a 0.5 mm diameter nozzle. The pressure of com-
37
pressed air for the flow of spray was adjusted to 1.9 bar. The inlet
temperature was maintained constant at 120 °C. A peristaltic
pump feed the spray dryer at a rate of 400 mL/h.
2.2.2. Experimental design
Feed suspensions were prepared from different formulations
according to a 2(k  p) Fractional Factorial Designs at 2 Levels. The
tested independent factors were rice starch (20–35%), gelatin (0–
1% starch basis) and CMC (0–1% starch basis) concentrations.
2.2.3. Analysis of spherical aggregates
2.2.3.1. Particle size analysis. The starch spherical aggregates size
distribution was analyzed by laser light scattering (Mastersizer X,
Malvern, UK) with a 300 mm lens. Starch powders were dispersed
with continuously mechanical agitation in isopropyl alcohol until
an obscuration of 11–15%. Three replicates of duplicate samples
(n = 6) measurements were recorded at 2 min intervals. Results
were expressed in terms of volumes occupied by particles 10%
undersize diameter (d0.1), mean size diameter (d0.5), 90% undersize
diameter (d0.9) and span index. Span was calculated as equation
(Eq. (1)).
d0:9  d0:1
Span ¼ ð1Þ
d0:5
2.2.3.2. Scanning electron microscopy (SEM) observation. Scanning
electron microscopy was used to observe the physical structure
of dried powders. Samples were fixed on metal pins with double-
sided tape, coated with a mixture of gold (95%) and palladium
(5%) by the plasma deposition method in a coater Polaron E5350
and observed in a Jeol JSM-5410 scanning microscope. Micropho-
tographs were obtained with an acceleration potential of 10 kV.
2.2.3.3. Porosity. Porosity and specific surface were measured with
a mercury porosimeter (AutoPore IV 9500 V1.07). Pore sizes were
calculated using Washburn equation (Eq. (2)) assuming that pores
were cylindrical in shape, the solid–liquid contact angle (u) is 130°
and the surface tension (c) of the mercury is 0.485 N/m.
 
1
D¼ 4c cos u ð2Þ
P
where D is the pore diameter and P the applied pressure for mer-
cury intrusion.
Intraparticle volume was calculated as the volume of mercury
intruded after the last inflection point of the intrusion/extrusion
curve (Palmer and Rowe, 1974).
2.2.3.4. X-ray powder diffraction measurements. The X-ray diffrac-
tion pattern of spray-dried powder and native rice starch was mea-
sured using Cu-Ka radiation produced by a Philips PW 1710
diffractometer. Starch powders (0.75 g) were packed tightly in
sample holders and exposed to X-ray beam generated at 40 kV
and 20 mA. The scanning region of the diffraction angle 2h was
from 5° to 30°.
38 S. Beirão-da-Costa et al. / Journal of Food Engineering 104 (2011) 36–42
3. Results and discussion
3.1. Particle size
Fig. 2 shows the SEM observation and particle size distribution
of spherical aggregates produced in tested formulations. As can be
observed in all tested conditions spherical aggregates are formed
even in the absence of bonding agents. Zhao and Whistler (1994)
refer the need of the presence of a bonding agent to ensure the
agglomerates formation. However, the protein content (0.64%) of
rice starch used in this study might be enough for spherules
production.
Starch concentration is the only parameter that significantly
(p < 0.05) affects the size (d0.1, d0.5 and d0.9) of formed aggregates
but gelatin also has a marginal effect on d0.1 (p = 0.077) (Eqs. (3)–
(5)). The presence of CMC, apparently, does not influence the
particle size. On the other hand, the presence of gelatin seems to
Fig. 2. Scanning electron microscopy microphotographs of spherical aggregates formed in all tested formulations. 500 Magnifications. Vertical bars indicate the volume of
each fraction size. White line shows the cumulative volume of successive fractions size.
render difficult the formation of aggregates as a higher fraction
of small particles, with sizes under 5 lm, corresponding to free
starch granules, is observed (Fig. 3).
d0:1 ¼ 2:20 þ 0:15S  2:90G  0:09S  CMC þ 0:06S  G  0:36CMC  G
ð3Þ
d0:5 ¼ 6:09 þ 0:24S  0:06CMC  1:26G  0:01S  CMC
þ 0:03S  G  0:85CMC  G ð4Þ
d0:9 ¼ 8:82 þ 0:47S þ 0:44G þ 0:09S  CMC þ 0:04S  G  3:19CMC  G
ð5Þ
The increase of starch concentration in feed suspensions leads
to a significant increase in spherical aggregates’ diameter. About
80% of formed aggregates from 35% of starch (w/w) suspensions
are under 30 lm diameter size, while in 20% of starch (w/w)
 S. Beirão-da-Costa et al. / Journal of Food Engineering 104 (2011) 36–42 39

Native Rice Starch

20% Rice Starch

35% Rice Starch

5 10 15 20 25 30
Diffraction Angle (2 θ )

Fig. 4. X-ray powder diffraction patterns for native and spray dried rice starch.

Native Rice Starch

20% Starch + 1% CMC

20% Starch + 1% Gel

35% Starch + 1% CMC

35% Starch + 1% Gel

20% Starch + 1% Gel + 1% CMC

35% Starch + 1% Gel + 1% CMC

5 10 15 20 25 30
Diffraction Angle (2 θ )

Fig. 5. X-ray powder diffraction patterns for native and spray dried rice starch in
the presence of bonding agents.

Fig. 3. Effect of starch and gelatine concentrations in feed suspensions on d0.1, d0.5
and span of produced spherical aggregates. r2 = 0.95; r 2adj = 0.80.

suspensions, 80% of aggregates are accounted by particles under

17 lm size. When bonding agents are present a slight reduction
in those diameters was observed.
Scattering of particles’ size, as measured by the span index, is Fig. 6. Effect of starch and gelatine concentrations in feed suspensions on degree of
also well described by the model (r2 = 0.97; r2adj = 0.91) and is crystallinity of produced spherical aggregates. r2 = 0.95; r2adj = 0.80.
40 S. Beirão-da-Costa et al. / Journal of Food Engineering 104 (2011) 36–42

mainly dependent on the presence of gelatin (p = 0.02) (Eq. (6)). To
starch and CMC concentrations only a marginal effect (p = 0.07 and
p = 0.09, respectively) on the heterogeneity of spherical aggregates
dimension could be attributed. When gelatin is present above
0.5% higher values of span were obtained confirming the higher
heterogeneity on spherical aggregates’ dimensions observed in
SEM microphotographs. This result could be relevant in further
studies of encapsulation, as the difference in diameters among
produced aggregates might influence the controlled release of core
materials.
Span ¼ 1:02 þ 0:06S  0:44CMC þ 0:62G þ 0:02S  CMC
 0:01S  G  0:17CMC  G
3.2. Crystalline structure
Starch, in its native form, shows a semi-crystalline structure
exhibiting amorphous and crystalline regions. When starch under-
goes changes, such as gelatinisation, this structure is affected and a
decrease in the degree of crystallinity is observed. The extension of
this loss is dependent on the intensity of the process.
X-ray diffraction patterns of spray-dried suspensions were com-
pared with the native starch. Figs. 4 and 5 illustrate the X-ray dif-
fractograms of native and spray-dried starch formulations. All
samples showed a typical A-type pattern, characteristic of cereal
starches, with strong reflections at 2h about 15° and 23° and an
ð6Þ unresolved doublet at 2h about 17° and 18°. Few small peaks were

Fig. 7. Exemple of mercury intrusion–extrusion curve (A) and pore size distribution (B) on rice starch spherical aggregates (20% Starch; 1% CMC; 1% Gelatine).
 S. Beirão-da-Costa et al. / Journal of Food Engineering 104 (2011) 36–42 41

Table 1
Porous spherules properties measured by mercury porosimetry.

Sample Total volume Average pore Intraparticle volume Intraparticle Total

(mL/g) diameter (lm) (mL/g) porosity (%) porosity (%)
20% Starch + 1% Gelatine 1.0965 2.9901 0.1104 10.1 55.69
20% Starch + 1% CMC 1.0936 3.4166 0.0918 8.4 57.54
20% Starch 1.1663 2.7469 0.0923 7.9 59.57
35% Starch 1.1322 3.2657 0.0954 8.4 58.58
35% Starch + 1% Gelatine 0.9155 3.0862 0.1957 21.4 50.66
20% Starch + 1% CMC + 1% Gelatine 0.9966 3.1491 0.0904 9.1 56.91
35% Starch + 1% CMC 1.0939 3.5032 0.1374 12.6 57.98
35% Starch + 1% CMC + 1% Gelatine 0.9453 2.9409 0.1449 15.3 51.86
27.5% Starch + 0.5% CMC + 0.5% Gelatine 1.2573 3.8492 0.1362 10.8 62.15

Fig. 8. Effect of starch and bonding agents concentrations on intraparticle porosity of produced spherical aggregates. r2 = 0.93; r2adj = 0.74.

also found at 2h of about 20° and 26°. The peak at 2h of about 20° is
suggestive of the presence of V-type complexes result from amy-
lose complexes with several substances. By comparing native rice
starch diffractograms with those of spray-dried starch without
bonding agents it can be observed that spray-drying of starch sus-
pensions did not induce alterations of crystal type and on peak
intensities (Fig. 4).
When binding agents were added to starch suspensions no new
peaks were observed in the diffractograms (Fig. 5). Nevertheless,
the shape and intensity of some peaks undergo small changes with
the presence of gelatin. When gelatin is added, less sharpened and
intense reflection peaks were observed mainly at 2h 17°, 18° and
26° which significantly (p = 0.050) influenced the degree of crystal-
linity of spray-dried powders.
A higher decrease in crystalline regions was observed when gel-
atin incorporation levels rise up to 0.4% (w/w) (Fig. 6) (Eq. (7)). De-
spite starch concentration apparently did not influence the
crystallinity of spray-dried powders, the effect due to addition of
gelatin is more pronounced for higher starch concentrations.
Crystallinity ¼ 75:99  0:43S  18:90CMC  2:26G þ 0:44S
 CMC  0:28S  G þ 3:14CMC  G
Results on samples crystallinity suggest also a certain degree of
starch structure modification, possibly like those induced by the
first stages of gelatinisation. Zhao and Whistler (1994) refer that
any condition that prevent starch gelatinisation seems to be
acceptable for spherules production. In the present work the inlet
drying temperature used was the same referred by those authors
however, a decrease of crystallinity occurs. As well, the observation
of the porous structures at a higher magnification (figure not
shown) shows a small fusion between some starch granules. With
these results we think that the drying temperature, despite the
short exposure time, induce the beginning of the gelatinisation
but, since the extension not significantly compromise granules
integrity, the creation of porous spheres can be achieved.
3.3. Porosity
A typical intrusion–extrusion curve of mercury porosimetry
measurements on rice starch spherules is illustrated in Fig. 7(A).
As the applied pressure increases, mercury will fill the existing
open pores. Larger pores will be filled at lower pressures while
higher pressure is necessary to completely fill the smallest ones.
A gradually intrusion of the mercury with increasing pressure at
the low pressure range can be observed, followed by a first abrupt
change in filling rate at about 30 psia. A sharp increase in volume is
indicative of the narrow particle size distribution of these poly-
mers samples (Palmer and Rowe, 1974). This aspect is corrobo-
rated, for all samples (data not shown) by the results obtained
for particle size distribution (Fig. 2).
At approximately 100 psia an abrupt shift of the filling rate is
ð7Þ
once more observed. This profile suggests the presence of both
interstitial voids (between spherules) and voids within particles
(intra-particle porosity). Some authors (Palmer and Rowe, 1974;
Webb, 2001) evaluate the total volume of the intra-particle voids
as the volume of mercury intruded after the last inflection point.
The pore size distribution of the samples (Fig. 7B) help to con-
firm the wideness observed in pore diameter. About 30% of all in-
truded mercury was held in pores, corresponding to the first
42 S. Beirão-da-Costa et al. / Journal of Food Engineering 104 (2011) 36–42
segment in the intrusion curve and, bringing into relation with
spherules size distribution, it is clear that these pores correspond
to interparticle voids. The largest amount of mercury, about 60%,
filled the pores with diameter ranging between 1 and 10 lm.
In all samples, hysteresis between intrusion and extrusion
curves was observed. This phenomenon is not uncommon since
it is observed in essentially all samples during mercury porosime-
try (Giesche, 2006). It also can be observed that, even after com-
plete depressurization, some mercury remains entrapped in the
porous spherules. This result is suggestive of pores with a throat
smaller than the pore cavity, ink bottle pores, and/or a network
of cylindrical open-ended cross-linked pores.
In Table 1 it can be seen the porous spherules characteristics
measured by mercury porosimetry. Starch and bonding agents’
concentrations did not significantly affect either the total porosity
of the samples or the average pore diameter. It was not found any
relationship between the formulation of the feed suspension and
these two parameters, as the model did not adjust to the experi-
mental data. However, it must be kept in mind that the average
pore diameter, as delivered by the equipment software includes
both inter and intra-particle voids and so may not represent what
is happening just with intra-particle pores, those that are really
effective for compound encapsulation. Otherwise, the encountered
differences on intra-particle porosity are explained by the model
(r2 = 0.93; r2adj = 0.74) (Eq. (8)). Starch and gelatin concentrations
are the only parameters that mainly affected the intra-particle
porosity (Fig. 8) being the effect of gelatin more pronounced at
higher levels of starch.
IPð%Þ ¼ 3:12 þ 0:18S þ 3:64CMC  4:28G  0:095G  CMC
þ 0:43S  G  5:85CMC  G
Nevertheless, along the intra-particle porosity evaluated as sug-
gested by Palmer and Rowe (1974) and Webb (2001) it should be
remarked that, considering the pore size distribution, a number
of intra-particle pores could not have been accounted as intra-par-
ticle voids. At the range of 2–6 lm, the section between the two
inflection points of the intrusion curve, some pores could be lo-
cated at the spheres and therefore the calculated intraparticle vol-
ume may be sub evaluated. The individualization among intra and
inter voids in this region is not possible.
4. Conclusions
The results of this study lead to a deeper knowledge on physical
characteristics of rice starch aggregates produced by spray drying.
It is possible to form starch spherules even in the absence of bond-
ing agents, nevertheless the presence of gelatin led to differences
in the formed structures. These differences are observed in both
particle size distribution and crystallinity of the spray-dried struc-
tures. More important than these aspects is the impact of starch
and gelatin concentrations on the structures’ internal porosity. A
higher internal void volume is achieved for higher concentration
of those matrix constituents, in the initial suspension. From the re-
sults, it may be also inferred that the role of gelatin on the system,
rather than a bonding action, is a structuring one.
Summarizing, when one intends to encapsulate in a starch with
small size granules, it is important to consider both the starch solid
content and the presence and concentration of these kinds of
agents, as the volume of voids available for encapsulation is
different.
Further studies are being conducted in order to evaluate also
the effect of these parameters on the protection degree of encapsu-
lated compounds.
Acknowledgements
The authors truthfully acknowledge to Drª Madalena Fonseca
from IICT and Profª Isabel Fonseca from (FCT-UNL) allowing per-
forming the X-ray diffraction determination and porosimetry mea-
surements, respectively. Also express their gratitude to Mr Octávio
Chaveiro from INIAP for the given support in microscopy studies.
Also thanks the financial support given by Portuguese Founda-
tion for Science and Technology (FCT) through the project PTDC/
AGR/ALI/67194/2006 and through a post doctoral grant of first
author (SFRH/BPD/44200/2008) supported by programme QREN
– POPH – Tipologia 4.1.
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