food and bioproducts processing 9 1 ( 2 0 1 3 ) 23–27

Contents lists available at SciVerse ScienceDirect

Food and Bioproducts Processing

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

Microencapsulation of passion fruit (Passiflora) juice with

n-octenylsuccinate-derivatised starch using spray-drying

Daniela Borrmann a,∗ , Anna Paola Trindade Rocha Pierucci b ,

Selma Gomes Ferreira Leite a , Maria Helena Miguez da Rocha Leão a
a Universidade Federal do Rio de Janeiro, Centro de Tecnologia, Bloco E, Escola de Química, Ilha do Fundão, Cidade Universitária, Rio de
Janeiro, Brazil
b Universidade Federal do Rio de Janeiro, Centro de Ciências da Saúde, Bloco J, Instituto de Nutrição, Ilha do Fundão, Cidade

Universitária, Rio de Janeiro, Brazil

a b s t r a c t

Food microencapsulation has been an efficient way of raising food shelf life during storage. In this work passion fruit
juice was encapsulated with n-octenylsuccinate-derivatised starch using a spray-dryer and stored at two different
temperatures. The shelf life of vitamin C was analysed and X-ray diffraction, scanning electronic microscopy and
laser diffraction analyses were performed. Samples stored at 7 and 25 ◦ C retained 77.1 and 71.5%, respectively, of
vitamin C after 77 days of storage. Capsules had an average size of 12.5 ␮m and were presented in an amorphous
form. n-Octenylsuccinate-derivatised starch showed to be an interesting material for the encapsulation of passion
fruit juice, and spray-drying proved itself as an inexpensive alternative to freeze-drying, capable of retaining vitamin
C during a long time of storage, and easy to be diluted in order to reconstitute the passion fruit juice for human
consumption.
© 2012 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Keywords: Microencapsulation; Spray-drying; n-Octenylsuccinate-derivatised starch; Passion fruit; Vitamin C

1. Introduction The production and commercialisation of passion fruit

Passion fruit (Passiflora) remains to the botanic family of Passi-
floraceae and is found in tropical climate. The plant has its
origin in North America, but is also spontaneous in Brazil,
Peru, Mexico, the Mediterranean region of Europe and North
Africa (Rain Tree Nutrition, 2011). In Brazil, 150 varieties are
known (Embrapa, 2011). Productivity in Brazil is high with
around 20–40 tons per hectare (IAC, 2011). Passion fruit is rich
in vitamin C, vitamins B1 and B2 and the pro-vitamin A, ␤-
carotene, as well as minerals such as K, P, Ca, Fe and fibres.
In the Food Composition and Nutrition Tables (Souci et al.,
2008) the following values are presented for 100 g of passion
fruit: 75.8% water, 63 kcal, 9.5 g carbohydrates, 0.4 g lipids, 2.4 g
proteins, 1.5 g dietary fibre, 3.9 organic acids and 0.9 g miner-
als. Vitamin C values have been reported as 40 mg in 100 g of
natural passion fruit juice (Suntornsuk et al., 2001).
juice has faced many difficulties regarding transport and shelf
life. The fruit spoils easily and needs to be commercialised
before it dehydrates. Concentrations of 14◦ Brix for natural
juice and 50◦ Brix for concentrated juice are considered safe
for commercialisation (IAC, 2011). A promising technology for
conservation and the increase of shelf life is microencapsu-
lation, defined as the packaging of solid, liquid and gaseous
material in sealed capsules of sizes between nanometres and
millimetres. The packaging isolates and protects the material
from ambient conditions such as light, temperature, oxy-
gen, humidity and from interaction with other substances.
If desired, the material can be released from the capsules
in a controlled way and under specific conditions (Dziezak,
1988; Risch, 1995; Ré, 1998). On the other hand, the ambi-
ent can also be protected from toxic encapsulated material
which could be a risk for health. Microencapsulation also

∗
Corresponding author. Tel.: +55 21 25627613.
E-mail address: borrmann@usp.br (D. Borrmann).
Received 17 January 2012; Received in revised form 19 July 2012; Accepted 1 August 2012
0960-3085/$ – see front matter © 2012 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.fbp.2012.08.001
24 food and bioproducts processing 9 1 ( 2 0 1 3 ) 23–27

protects material from evaporation (Jackson and Lee, 1991). chamber wall. n-OSA starch does not possess a proper taste
In food systems, microencapsulation can be utilised for acids, and therefore does not influence the taste of the final product.
lipids, enzymes, microorganisms, flavours, vitamins, miner- As a comparison, pure n-OSA starch has been diluted in
als, growth agents and colorants (Bakan, 1973; Pothakamury water to a concentration of 10% and been processed by spray
and Barbosa-Cánovas, 1995). There are many methods of drying, under the same conditions as the juice samples.
encapsulation with their main difference in the combination
of the encapsulating material and the nucleus, which can be
2.2. Shelf life analysis by vitamin C stability
of physical, chemical or physicochemical nature (Shahidi and
Han, 1993; Gouin, 2004).
The shelf life of the capsules was evaluated by vitamin C anal-
For several decades, microencapsulation has been per-
ysis during 77 days.
formed with the help of spray drying and used widely in
Vitamin C is easily degraded by oxidation and is therefore
the food industry, since it is a rather inexpensive method
used as a chemical control of sample stability. It represents a
(Gouin, 2004). The encapsulating agent should not react
useful indicator of the efficiency of the encapsulating material
with the nucleus. The most common materials used for
as a nutrient and vitamin protector. The capsules were stored
microencapsulation by spray-drying are gums, like gum ara-
in well-closed Falcon tubes and submitted to different tem-
bic, low-molecular-weight carbohydrates like maltodextrins
peratures and storage times. Samples were divided into two
and saccharose, cellulose, gelatine, lipids and proteins, like
parts. One part was stored at ambient temperature of 25 ◦ C
soy proteins (Gharsallaoui et al., 2007; Fäldt and Bergenståhl,
and the second part in a refrigerator at 7 ◦ C. Storage was per-
1995; Hogan et al., 2001a,b,c; Kim and Morr, 1996; Keogh et al.,
formed in duplicates at each temperature. All samples were
2001; Lin et al., 1995).
maintained in the dark during 77 days. Samples were ana-
A common material for microencapsulation in food indus-
lysed six times on the course of 77 days in triplicate, following
try is n-octenylsuccinate-derivatised starch, a modified starch.
the method of Tillmans, according to the Analytic Norms of
Its modification consists in the addition of a lipophylic compo-
the Adolfo Lutz Institute (1985). This method is based on the
nent, octenylsuccinate, which increases the emulsion stability
strong reduction capacity of vitamin C, which reduces 2-6-
(Arburto et al., 1998). n-Octenylsuccinate-derivatised starch is
diclorophenol-indophenol.
used by the food and pharmaceutical industry with approval of
the FDA as food additive since the content of octenyl-succinate
does not exceed 3% (Bastos et al., 2009). 2.3. X-ray diffraction
The aim of this work was to create stable capsules of pas-
sion fruit juice with the aid of n-octenylsuccinate-derivatised Measurement of the degree of crystallinity of the samples
starch, using the spray-drying technology and to characterise was performed in an X’Pert Pro Diffractometer (PANalytical,
the capsules with respect to their size, surface morphology Almelo, The Netherlands) in triplicates, after 25 days of stor-
and crystallinity. The stability of the capsules was tested by age. Capsules were dissolved in ethanol prior to analysis. A
vitamin C analyses during 77 days of storage at two different sample of pure n-OSA starch was also measured in order to
temperatures. compare it to the samples. The degree of cristallinity was
obtained by comparison of the peak areas between sample
and control sample.
2. Methods

2.1. Production of passion fruit microcapsules with
n-octenylsuccinate-derivatised starch (n-OSA starch)
Passion fruits were acquired at local markets in Rio de Janeiro.
Fruits were washed; the juice was obtained through a com-
mercial food processor and filtered through qualitative filter
paper in order to eliminate solids in the suspension. Then n-
OSA starch (National Starch, USA) was added to the amount
of 10% (10 g of n-OSA starch in 100 mL of juice) and homogeni-
sation was performed manually by stirring. Subsequently,
the mixtures were spray-dried in a Büchi Mini Spray Dryer
B290, at an inlet air temperature of 180 ◦ C, feed temperature
25 ◦ C and a feed flow rate of 6 mL/min (maximum capacity
30 mL/min). The yield of that method is of about 50–60% of
initial quantity. The outlet temperature was maintained at
approximately 80 ◦ C. These conditions have been chosen after
preliminary trials with different conditions and consultancy
of previously published literature. The concentration of 10%
of n-OSA starch was found to be the least value necessary in
order to avoid excessive powder stickiness on the chamber
wall during spray-drying. Below 10%, the process yield was
unsatisfactory. n-OSA starch is known to be a good support
material in order to elevate the glass transition temperature
of juices, which are usually very low and make it impossi-
ble to spray-dry because the juice would get stuck on the
2.4. Scanning electronic microscopy
Characterisation of the microstructure of the microcapsules’
surface was performed in a JSM-5460LV Scanning Electron
Microscope (JEOL, Tokyo, Japan) following the methodology
described by Sheu and Rosenberg (1998). Microcapsules were
fixed in aluminium stubs using double-coated carbon con-
ducting adhesive tapes. Samples were then sputter coated
with gold and analysed. The methodology allows visualising
the structure of the microcapsules and their integrity (Shahidi
and Han, 1993).
2.5. Laser diffraction
The particle size was analysed in a Mastersizer 2000 Laser
Diffraction Particle Size Analyzer with a Hydro 2000S sample
dispersion unit (Malvern, Worcestershire, UK). Samples were
analysed by light scattering after dilution in n-butyric alcohol.
2.6. Statistical analysis
Obtained data were compared by variance analysis at p < 0.05.
Differences between the means were determined with the
Tukey multiple test.
 food and bioproducts processing 9 1 ( 2 0 1 3 ) 23–27 25

3. Results and discussion

3.1. Production of passion fruit microcapsules with

60

[c] of vitamin C in µg/mL

n-OSA starch

The mixture of fresh filtered passion fruit juice with 10% of 40

n-OSA starch was spray-dried and resulted in a white, slightly
yellowish powder, easy to be diluted in cold water in order to
reconstitute the juice for consumption.
It is important to consider that the addition of 10% of n-OSA
starch to the passion fruit juice leads to a significant increase
in the energy value of the resulting product. Since the natu-
ral passion fruit juice has a very low energy value of around
60 kcal/100 g, and a solid content of about 15 g/100 g, the addi-
tion of 10 g of n-OSA starch adds about 45 kcal/100 g to the
capsules and therefore significantly increases the dry weight
of the product. However, a lower amount of n-OSA starch did
not result in a complete encapsulation of the passion fruit
juice and therefore this calorie increment needs to be accepted
for the present objective. On the other hand, in former exper-
iments where the passion fruit juice was encapsulated using
the method of freeze-drying, the necessary percentage of n-
OSA starch was 20% (Borrmann et al., 2011). In this case, the
dry weight of the product was approximately doubled, which
shows, that the present method of encapsulation by spray-
drying leads, besides other advantages of the methodology, to
a lower calorie product.
3.2. Shelf life analysis by vitamin C stability
Encapsulated passion fruit samples were stored at 7 and 25 ◦ C,
in the dark, for 77 days. During this time samples were ana-
lysed for vitamin C content in triplicates. All samples stored at
7 and 25 ◦ C maintained their physical appearance during the
time of storage, presenting a homogeneous powder.
Microencapsulated samples showed a significant loss of
vitamin C concentration (Fig. 1), however this loss is much
lower than the one in samples freeze dried and analysed pre-
viously (Borrmann et al., 2011). Degradation of the spray-dried
samples was less intense and more delayed. At 7 ◦ C and 25 ◦ C,
77.1 and 71.5% of the vitamin, respectively, were not degraded.
These results show the efficiency of n-OSA starch as a vitamin
20 7ºC
25ºC
0
0 20 40 60 80
days of storage
Fig. 1 – Vitamin C concentration in samples of passion fruit
juice, encapsulated in n-OSA-starch, spray-dried and
stored in the dark at 7 and 25 ◦ C during 77 days. Standard
deviations have been insignificant (p < 0.05; data not
shown).
C protector during 77 days of storage. Here it is shown that the
storage temperature has only a small influence on the vita-
min C degradation. When samples are dried in a spray-dryer
and together with a low storage temperature, the main part
of the vitamin C can be preserved during a very long time.
However, compared to formerly obtained results, where pas-
sion fruit juice was freeze-dried with n-OSA starch, the spray
drying seems to confer a higher vitamin C protection than
freeze-drying (Borrmann et al., 2011).
3.3. X-ray diffraction
The degree of crystallinity of the samples was analysed by
X-ray diffraction. The encapsulated passion fruit juice and a
sample of pure n-OSA starch were measured (Fig. 2) after 25
days of storage. Images have proved, as expected, that both,
n-OSA starch and the capsules of passion fruit juice are rep-
resented in an amorphous, disorganised form. n-OSA starch
usually shows a small tendency of crystallisation, represented
by the peaks in the graph, which is reduced when mixed
with the passion fruit juice, leading to a more amorphous

2500 (a) (b)

2000
2500
Intensidade

1500 2000
Intensidade

1500
1000

1000
500
500

0
10 20 30 40 50 60 70 80 0
20 40 60
2θ 2θ

Fig. 2 – Image of X-ray diffraction of an encapsulated sample of passion fruit juice in n-OSA starch (a) and a sample of pure
n-OSA starch (b).
26 food and bioproducts processing 9 1 ( 2 0 1 3 ) 23–27
Fig. 3 – (a) Scanning electronic microscopy of passion fruit
juice encapsulated in n-OSA starch, at a magnification of
1000×. (b) Scanning electronic microscopy of passion fruit
juice encapsulated in n-OSA starch, at a magnification of
3000×.
sample, with no peaks accusing crystallisation. This is par-
ticularly interesting, since usually amorphous samples tend
to be very hygroscopic and to absorb water during storage.
Samples then become sticky and form agglomerates as the
amorphous sugars are transformed into crystalline sugars in
order to reach an energetically more stable state. This charac-
teristic prejudices the storage of the samples since the water
absorption implicates in weight gain and vitamin C degra-
dation, microstructure collapse and potential microbiological
instability, for example. Nevertheless, in this work, samples of
encapsulated passion fruit juice maintained their amorphous
state during 25 days and remained as a loose and dry powder,
which guarantees vitamin C stability.
3.4. Scanning electronic microscopy
With the help of scanning electronic microscopy it was possi-
ble to physically characterise the surface of the passion fruit
juice microcapsules. Measurement was performed at mag-
nifications of 55×, 1000× and 3000× (Fig. 3a and b). As the
samples have been spray-dried, they show the typical micro-
sphere formation, at different sizes, due to the passage of the
samples through the spray-dryer. Microspheres are of a very
small micrometer size.
Fig. 4 – Image of laser diffraction analysis of the
microcapsules of passion fruit juice in n-OSA starch.
3.5. Laser diffraction
The particle size analysis by laser diffraction resulted in a
mean size of 12.5 ␮m (Fig. 4). This result proves that the present
capsules can be considered microcapsules since their diame-
ter is of micrometer size. The figure shows that the particles
have very similar sizes, which means that the powder is very
homogeneous. These results had already been expected, since
the procedure of spray drying leads to very small micrometer
size particles.
4. Conclusions
Passion fruit juice showed to be compatible to encapsulation
with n-OSA starch, which is an inexpensive material easy to
be obtained, and with optimum properties for its use in the
food industry. n-OSA starch does not alter the passion fruit
taste and aroma, and is easy to be diluted in cold water after
spray-drying and storage. Spray-drying of passion fruit juice
encapsulated in n-OSA starch results in very small and stable
microcapsules, in the form of a homogeneous white powder.
Furthermore, this work has shown that n-OSA starch is an
excellent vitamin C protector, capable of retaining almost all
the vitamin C present in the samples during a long storage
time. Once encapsulated, the passion fruit can be transported
and stored in its powder form until reaching its destination
for further industrialisation, without suffering significant loss
of nutritional properties. The obtained powder preserves a
strong and pleasant smell of passion fruit and the juice is easy
to be reconstituted. These parameters will be studied further
by sensory analyses in order to test consumers’ acceptance.
Acknowledgement
We thank CNPq for financial support and researcher’s schol-
arship.
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