Journal of Microencapsulation, December 2008; 25(8): 549–560

Microencapsulation of avocado oil by spray drying using

whey protein and maltodextrin

E. K. BAE1 & S. J. LEE2

1
Plant Resources Research Institute, Duksung Women’s University, Seoul, Korea and 2Institute of Food, Nutrition and
Journal of Microencapsulation Downloaded from informahealthcare.com by Columbia University on 04/05/13

Human Health, Massey University, Auckland, New Zealand

(Received 12 November 2007; accepted 18 March 2008)

Abstract
Cold pressed avocado oil was microencapsulated by spray drying in four different wall systems consisting of whey protein isolate
(WPI) alone or in combination with maltodextrin (MD) DE 5 at various ratios (90 : 10, 50 : 50 and 10 : 90). The WPI only or WPI/
MD (90 : 10) powders were spherical and smooth, whereas the WPI/MD (50 : 50 and 10 : 90) powders exhibited pronounced
surface collapse. Increasing the MD ratio resulted in higher bulk density and wettability, probably due to more compact physical
structure and hydrophilic wall matrix. Surface free oil contents and microencapsulation efficiencies of powders were 11–16% and
45–66%, respectively, and no significant differences were observed between the samples. The crude avocado oil used in this study
For personal use only.

appeared to be stable against oxidation at cold and ambient temperatures, irrespective of microencapsulation. However, at high
temperature of 60 C, the oxidative stability decreased significantly in all cases but it was improved to some extent by
microencapsulation.

Keywords: Microencapsulation, spray drying, avocado oil, oxidative stability, whey protein, maltodextrin

Introduction because of its high absorption and penetration ability

Cold pressed avocado oil produced in New Zealand
has been increasingly attracting the interest of health
conscious consumers since it has unique flavour, taste
and green colour and contains a high concentration
of oleic monounsaturated fatty acid, 70% and
substantial amounts of health beneficial compounds,
such as antioxidant vitamins and phystosterols, for
instance -tocopherol, -carotene, lutein and
-sitosterol (Requejo et al. 2003). Monounsaturated
fatty acid and phytochemicals are known to provide
various positive health effects on serum cholesterol
and lipoproteins, coronary heart disease, cancer,
diabetes and prostate (Human 1987, Swisher 1988,
Requejo et al. 2003). As a result, avocado oil is
accepted as healthy oil and recommended to include
in diets for direct human consumption (Swisher 1988,
Gurr 1992). Besides its use in foods, avocado oil has
also been identified as one of the most beneficial
plant oils in pharmaceutical and cosmetic products
into skin and biological properties (Human 1987,
Swisher 1988).
Most edible oils, however, are chemically unstable
and susceptible to oxidative deterioration, especially
when exposed to oxygen, light, moisture and tempera-
ture. The instability and susceptibility of edible oils to
oxidative degradation result in a loss of nutritional
quality and a development of off flavours, hence
affecting shelf stability and sensory properties of
products (Velasco et al. 2003). To suppress or retard
lipid oxidation and increase a range of applications,
edible oils or fats have been microencapsulated.
Microencapsulation is a technique of enclosing liquid
droplets or small particles of a sensitive substance
(called core) within a continuous thin film or coating
material or embedding in a solid matrix of polymers
(referred to as wall or carrier) (Dziezak 1988). Among
the microencapsulation methods, spray drying is the
most commonly employed technique used in the food
industry (Rosenberg et al. 1990, Shahidi and Han 1993,

Correspondence: Sung Je Lee, Institute of Food, Nutrition and Human Health, College of Sciences, Massey University, Private Bag 102904, North Shore Mail
Centre, Auckland, New Zealand. Tel.: 64-9-414-0800 ext 41161. Fax: 64-9-443-9640. E-mail: s.j.lee@massey.ac.nz

ISSN 0265–2048 print/ISSN 1464–5246 online ß 2008 Informa UK Ltd.

DOI: 10.1080/02652040802075682
 550 E. K. Bae & S. J. Lee
Drusch et al. 2006) as it is simple, easy and cheap to use
(Drusch et al. 2006). Besides, spray drying transforms a
liquid into a solid form, allowing easy handling, storage
and transportation and uniform mixing and dispersion
in food formulations when small quantities need to be
incorporated (Shahidi and Han 1993, Tan et al. 2005).
In the oil microencapsulation process by spray
drying, one of the prerequisites is to prepare a stable
emulsion with proper chemical and physical properties
since emulsion stability, properties and composition
determine heavily the quality attributes of spray dried
oil encapsulated powders, such as surface free oil
content, microencapsulation efficiency, structure, oxi-
dative stability and physical properties (flowability,
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bulk density and dispersibility). Generally, an emulsion
ideal for oil encapsulation should have the following
properties: small size and narrow distribution of oil
droplets stable to agglomeration and coalescence, a
high solid content for enabling to form a continuous
matrix as a protective barrier where oil droplets are
uniformly distributed and embedded, a low viscosity for
easy flow, pump and spray and a proper ratio of wall
solids-to-oil. It is therefore important to characterize
the properties of emulsions that could be affected by
type and composition of wall and oil materials, which in
For personal use only.
turn affect the subsequent spray dried emulsions.
Numerous wall materials have been studied and used
for their suitability as encapsulating agents in spray
drying. Wall materials for microencapsulation of oils by
spray drying have emulsifying properties, high water
solubility, low viscosity and film-forming and drying
properties (Young et al. 1993a, Sheu and Rosenberg
1995, Re 1998, Kagami et al. 2003). Typical wall
materials include proteins (sodium caseinate, whey
proteins, soy proteins and gelatin) and hydrocolloids
(modified starch and gum arabic). Among proteins,
whey proteins have been shown to be an excellent
encapsulating agent for microencapsulation of oils/fats
and volatiles (Reineccius 1988, Sheu and Rosenberg
1995, Keogh and O’Kennedy 1999, Moreau and
Rosenberg 1999, Kagami et al. 2003). Hydrolysed
starches (glucose, lactose, corn syrup solids and
maltodextrin) are generally added as a secondary wall
material (a filler) to improve drying properties of
sprayed droplets by enhancing the formation of dry
crust around drying droplets and increase the oxidative
stability of encapsulated oils by reducing oxygen
permeability of wall matrix (Sheu and Rosenberg
1995, Kagami et al. 2003). However, one problem
related to these components is their high susceptibility
to form crystalline form as they have very low
glass transition temperatures. Crystallization of
carbohydrates via glass transition causes disruption of
structural integrity of wall matrix and induces agglom-
eration or caking of powders, resulting in the release of
some encapsulated oil and induction of lipid oxidation
(Drusch et al. 2006). In this regard, relatively larger
molecular weights of maltodextrins (MD) with low
dextrose equivalent (DE) values, that have much higher
glass transition temperatures, confer better physical
stability to wall matrix systems (Beristain et al. 2002,
Fuchs et al. 2006).
Microencapsulation of various types of oils by spray
drying has been attempted for not only protection from
oxidation but also more diversified applications of oils
in food products. However, to the authors’ knowledge,
there are no reports studied on encapsulation of
avocado oil by spray drying. The objectives of this
study were therefore to produce avocado oil encapsu-
lated powders by spraying drying using wall systems
consisting of whey protein isolate (WPI) and maltodex-
trin (MD) DE 5 at various ratios and investigate the
effects of different wall systems on structure and
physical properties of the powders and oxidative
stability of the encapsulated avocado oil during storage.
Materials and methods
Materials
Whey protein isolate (WPI) containing 97% protein
was supplied by Fonterra NZ Ingredients (Whareora,
New Zealand). Maltodextrin (MD) with a DE value of
5 produced by Tate & Lyle Ingredients Americas Inc
(Decatur, IL) was purchased from Bronson and Jacobs
Pty. Ltd. (Auckland, New Zealand). Both WPI and
MD were used as encapsulating wall materials. Extra
virgin, cold pressed avocado oil was supplied by
Olivado New Zealand Ltd. (Kerikeri, New Zealand)
and used as a core material. All chemicals used were of
analytical grade.
Microencapsulation by spray drying
Emulsion preparation. Wall solutions containing
20% (w/w) total solids were prepared with WPI alone
or WPI/MD mixtures at different proportions of 90 : 10,
50 : 50 and 10 : 90 on dry weight by dissolving in
distilled water containing 0.02% (w/w) of sodium
azide as a preservative. Emulsions and spray dried
emulsions corresponding to each of these wall solutions
are thereafter denoted W100, W90MD10, W50MD50
and W10MD90, respectively. Crude avocado oil
warmed to 40 C was added into each wall solution
held at 40 C at a proportion of 50% (w/w) of the wall
solids. This means that in all cases the ratio of oil-
to-wall solids in emulsions was 33.3 : 66.7 on dry weight
basis. The mixtures were homogenized using a mechan-
ical homogenizer (VirTishear Tempest model, The
VirTis Company, NY) at 13 000 rpm for 2 min and
then at 22 000 rpm for 10 min.
Spray drying. The emulsions prepared were spray-
dried with a small scale spray dryer (Model SL10,
Saurin Group of Companies, Port Melbourne,
Australia) equipped with a twin fluid nozzle operated
 Microencapsulation of avocado oil by spray drying
at air pressure of 400 kPa. The dryer had an evapora-
tion rate of 1 kg h1. The dimensions of the dryer were
1.4, 0.8 and 1.0 m for height, width and length,
respectively. In order to maintain homogeneity and
prevent coalescence of oil droplets while fed into the
spray dryer, the emulsions were gently stirred using a
magnetic stirrer. The inlet and outlet air temperatures
used were 180 and 80 C, respectively. The dried
powders were stored in airtight glass jars wrapped in
an aluminum foil at 4 C until analysis.
Particle size and size distribution of emulsions
The size and size distribution of oil droplets in each
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emulsion were measured at 25 C with a Malvern
MasterSizer MSE (Malvern Instruments Ltd.,
Worcestershire, UK). The parameters used for analysis
of the size distribution were defined by the presentation
code 2NAD. The relative refractive index (N), which
was the ratio of refractive index of the emulsion particle
(1.456) to that of the dispersion medium (1.33), was
1.095. The absorbance value of the oil droplets
was 0.001. The sizes reported are volume weighed
mean diameters D(4,3) which are defined as
P
ni d 4i =ni d 3i , where ni is the number of droplets with
For personal use only.
diameter di.
Emulsion viscosity
Viscosities of the emulsions were analysed as a function
of shear rate using a rheometer (AR550, TA
Instruments Ltd., Leatherhead, Surrey, UK) equipped
with a cone and plate geometry. The rotating cone was
60 mm in diameter and the cone angle was 2 .
All measurements were carried out in a temperature-
controlled vessel at 25 C. The data were plotted in the
logarithmic scale on viscosity as a function of
shear rate.
Microscopic examination of emulsions
The emulsions were examined visually with a light
microscope (HBO 50/AC, Carl Zeiss Inc., Göttingen,
Germany). A few drops of the emulsion samples were
mixed with distilled water and then placed on a glass
slide covered with a cover slip and observed under the
microscope. Microscopic images were taken using a
digital camera attached to the microscope.
Compositional analyses
The moisture content of the powders was measured
gravimetrically by drying 2 g of the powder samples in
an air oven at 105 C for 12 h. The total oil content of
the powders was determined gravimetrically by ether
extraction according to the Rose–Gottlieb method
(Bradley et al. 1993) and expressed as the percentage
per 100 g of powder.
551
Powder bulk density
Bulk density of the powders, which is defined as the
weight of a given volume of powder, was determined
according to the tapping method described by
Beristain et al. (2001) with some modifications.
Approximately 0.5 g of the powders were loosely
placed into a 5 ml measuring cylinder. The cylinder
was tapped on a flat surface by hand until a constant
volume was obtained. The bulk density was calcu-
lated by dividing the sample weight by the volume
and expressed in g cm3.
Powder wettability
Wettability of the powders was determined using the
method of Fuchs et al. (2006). One gram of the powders
was sprinkled over the surface 100 ml of distilled water
at 20 C without agitation. The time taken for the
powder particles to sediment or sink or submerse below
and disappear from the surface of water were measured
and used for a relative comparison of the extent of
wettability between the samples.
Surface free oil content and microencapsulation
efficiency
The amount of unencapsulated oil (i.e. free oil or
surface oil) present at the surface of the powders was
measured using a method described by Tan et al.
(2005) with some modifications. Fifteen millilitres of
hexane was added to 2 g of powder in a 30 ml glass
vial with a screw cap and shaken with a vortex mixer
for 2 min at ambient temperature to extract free oil.
The solvent mixture was then decanted and filtered
through a Whatman No. 1 filter paper. The collected
washed powder on the filter paper was rinsed three
times with 20 ml of hexane at each time by passing it
through the powder. The residual powder was then
dried to vaporize all residual solvent at 60 C to a
constant weight. The free oil content was then
calculated as percentage by the weight difference in
the powder before and after extraction and washing
with hexane. Microencapsulation efficiency (ME) was
calculated using the following formula: ME ¼ [(Total
oil – Surface oil)/Total oil]  100.
Oxidative stability of encapsulated oil
To determine the oxidative stability of encapsulated
oils over storage time, samples of each powder (30 g)
were placed in airtight glass bottles and the bottles
were stored in an incubator at 4, 25 or 60 C for
up to 8 weeks. The oxidative stability was monitored
by measuring the peroxide values (PV) of oils
extracted from the powders. At weekly intervals, 1 g
of each sample was withdrawn from the bottles. For
oil extraction, the withdrawn samples were dispersed
into 4 ml of warm distilled water (40 C) in glass tubes
followed by vortexing for 2 min. The mixtures were
 552 E. K. Bae & S. J. Lee
then added and extracted with 45 ml of hexane/iso-
propanol (3 : 1, v/v) by shaking vigorously for 15 min
using an orbital shaker at 400 rpm. The tubes were
centrifuged at 3000 rpm for 2 min. The organic
solvent phase was collected and heated at 70 C for
evaporation and the remaining extracted oil sample
was collected for the subsequent assay for PV. In all
cases, the bulk avocado oil (i.e. unencapsulated oil)
was also stored and analysed under the same
conditions.
The colourimetric method described by Hardas
et al. (2000) was used with some modifications. The
extracted oil (0.03–0.04 g oil) was added to 7.96 ml
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of chloroform/methanol (7 : 3, v/v) mixture in a glass
tube, followed by the addition of 20 ml each of
ammonium thiocyanate and ferrous chloride solu-
tions. The final mixture was then mixed and
incubated for 5 min in a dimmed light at ambient
temperature. After incubation, the absorbance was
measured with a UV/vis spectrophotometer (Model
UV-1601, Shimazu Corporation, Tokyo, Japan) at
505 nm. Reagent and oil blank assays were also
carried out. PV was quantified using a standard curve
created from a series of hydrogen peroxide standard
solutions and expressed as milliequivalents (meq)
For personal use only.
hydroperoxide per kg of oil.
Scanning electron microscopy of powders
Microstructural features of the spray dried avocado
encapsulated powders were analysed by scanning
electron microscopy (SEM). The powder samples
were mounted on SEM stubs using a double-sided
adhesive tape. The sample specimens were subse-
quently coated with a thin layer of platinum in a
vacuum evaporator using a sputter coater (Polaron
SC 7640, Polaron, Hertfordshire, UK). The coating
current and voltage used were 5–10 mA and 1.1 kV.
The sputter coated samples were then visualized at a
voltage of 5 kV with a SEM (Philips XL30S FEG,
Eindhoven, The Netherlands) equipped with an
EDS detector (SiLi, Lithium drifted with a Super
Ultra Thin Window). The SEM micrographs repre-
senting the microstructure of the powders were taken
using software installed on a PC connected to the
system.
Table I. Volume mean size (D4,3) and specific surface area of oil droplets in avocado oil emulsions prepared at different ratios of WPI-to-MD
DE 5 at a given concentration of avocado oil.
WPI/MD
Emulsion ratio
W100 10 : 0
W90MD10 9:1
W50MD50 1:1
W10MD90 1:9
a,b,c
Different letters within each column are significantly different at p 5 0.05.
Statistical analysis
The results obtained were analysed using an analysis of
variance (ANOVA) with MinitabÕ Release 14.1 statist-
ical software. Significance was established at p 5 0.05.
Results and discussion
Particle size and size distribution of emulsions
Avocado oil emulsions were prepared at a given oil
concentration using four different formulations con-
sisting of either WPI alone or WPI/MD mixtures at
three different ratios. The volume weighed mean
particle sizes (D4,3) and specific surface areas of oil
droplets measured were in the range of 2.27–4.01 mm
and 5.58–8.20 m2 ml1, respectively (Table I). They
were found to be affected by the WPI-to-MD ratio.
The smallest particle size was observed in the emulsion
containing WPI only as wall material. Increasing the
MD proportion from 0 to 90% by replacing the same
amount of WPI resulted in a gradual increase in the
particle size of the emulsion oil droplets. Interestingly, a
high correlation was found to exist between the
amounts of MD and the emulsion particle sizes
(R2 ¼ 0.98). A similar trend of increasing particle size
of oil droplets was shown by Hogan et al. (2001b) when
the ratio of sodium caseinate to MD DE 28 in
emulsions decreased, although the extent of changes
was much smaller than these results. WPI has excellent
emulsifying properties while MD shows a lack of
surface binding activities at oil/water interfaces.
The larger oil droplets observed at the higher MD
ratio could thus be explained by a reduced emulsifying
capacity of the emulsions derived from the lower
amount of WPI. Like it is depicted in Figure 1, the
size distributions of oil droplets appeared to be broad in
all cases, ranging from 0.1–15 mm, but revealed two
distinct patterns that could be attributed to the different
ratios of WPI-to-MD. The emulsions of W50MD50
and W10MD90 showed a bimodal type of particle
distribution in which large particle sizes had much
higher proportions than small particle sizes. In contrast,
the other two emulsions of W100 and W90MD10
exhibited a unimodal distribution.
It should, however, be mentioned that since the
amount of WPI available in all emulsion systems was
Oil/WPI Specific surface
ratio Size (mm  SD) area (m2 ml1  SD)
0.5 : 1 2.27  0.02a 8.20  0.05a
0.56 : 1 2.29  0.00a 8.11  0.00a
1:1 3.10  0.00b 6.78  0.00b
5:1 4.01  0.01c 5.58  0.01c
 Microencapsulation of avocado oil by spray drying 553

believed to be sufficient enough to enable them to cover
all newly created oil droplet interfaces, the differences in
droplet sizes between the emulsions and their overall
rather large mean sizes might also be accountable to a
rather low homogenization pressure employed in this
study by using a shear type of homogenizer which is less
efficient in producing a fine emulsion than does a high
pressure homogenizer.
Emulsion stability, in terms of flocculation, coales-
cence or phase separation, has been reported to have an
influence on microencapsulation efficiency, stability
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and properties of spray dried oil powders (Tan et al.
2005). Therefore, after preparation of the emulsion it
must remain stable during the spray drying process.
In the present study, the time taken to complete the
spray drying process for one batch after emulsion
preparation was 30–40 min during which no signifi-
cant changes in emulsion stability had been observed in
the preliminary studies (no data shown). Microscopic
pictures of the emulsions are shown in Figure 2. It
confirms that the emulsion oil droplets were distributed
and suspended uniformly in the aqueous phase without
noticeable flocculation or separation in all cases.

Emulsion viscosity
8
7 W100
The emulsions were measured for their viscosities to
W90MD10 find out an effect of the different ratios of WPI-to-MD
6
W50MD50 which may ultimately influence the properties of the
Volume (%)

5 W10MD90
resultant powders. The results shown in Figure 3
4 indicated that the viscosities were affected by the
3 WPI-to-MD ratios although the differences were
2 small. It was not possible to determine whether such a
minor but apparent difference in viscosity could have
1
an impact on drying process as to the formation and
0 properties of powder particles. The emulsion (W100)
0.1 1 10 100
prepared with WPI alone demonstrated the lowest
For personal use only.

Size of emulsion oil droplets (µm)

Figure 1. Particle size distributions of oil droplets in
avocado oil emulsions prepared at different ratios of
WPI-to-MD DE5.
viscosity whereas the highest viscosity was observed in
the W10MD90 emulsion which had the highest
MD ratio. The higher viscosity with the higher MD

Figure 2. Light microscopic images (at 400 magnification) of emulsions in which avocado oil was emulsified in different wall
solutions containing WPI alone or in combination with MD DE 5 at different ratios. (a) W100, (b) W90MD10, (c) W50MD50
and (d) W10MD90.
 554 E. K. Bae & S. J. Lee
ratio was probably due to the fact that the MD DE5
with a low DE used contains a large amount of long
straight- and branched-chain units which might exhibit
some viscosity characteristics as do starches. All
emulsions tested had the Newtonian fluid behaviour
although the viscosities—except for the W100 emul-
sion—appeared to decrease slightly with increasing
shear rate. This phenomenon might be resulting from
the presence of some flocculated oil droplets becoming
segregated during the viscosity measurement, which
could be possibly formed as the viscosity was not
measured immediately after the emulsion preparation.
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Microencapsulation efficiency
One of the important quality parameters in encapsula-
tion of oils by spray drying is microencapsulation
efficiency (ME), that is the percentage of encapsulated
oil in total oil. The ME is commonly determined
indirectly by extracting unencapsulated oil (i.e. free oil)
present on the surface of microcapsules through
washing powders with an organic solvent (Velasco
et al. 2003). The presence of free oil influences adversely
the physical properties of spray dried powders, such as
flowability, bulk density and dispersibility, and induces
more rapid lipid oxidation (Granelli et al. 1996, Keogh
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et al. 2001). It should be noted that the free oil analysis
0.100
W100
W90MD10
Apparent viscosity (Pa.s)
W50MD50
W10MD90
0.010
0.001
1 10
Shear rate (s−1)
Figure 3. Viscosity flow curves plotted as a function of shear
rate obtained from avocado oil emulsions prepared at
different WPI-to-MD DE5 ratios.
Table II. Moisture and free oil contents and microencapsulation efficiency of different batches of spray dried avocado oil
powders prepared with encapsulating wall materials of WPI and MD DE5 at different ratios.
Powder wall system WPI/MD ratio
W100 10 : 0
0W90MD10 9:1
W50MD50 1:1
W10MD90 1:9
by solvent extraction can also induce an extraction of
encapsulated oil to some extent from the near surface of
microcapsules (Buma 1971, Vega and Roos 2006),
thereby resulting in a higher free oil content than an
actual content.
Table II shows that the free oil contents measured
were in the range of 11.39–15.75% and the levels of ME
were 45–66%. No significant differences between the
samples were found (p 4 0.05). This means that the free
oil contents (or ME values) were not correlated directly
with the ratios of WPI to MD or the emulsion oil
droplet sizes. The former also implies that the partial
replacement of WPI by MD did not increase the ME of
the powders. The moisture contents of the powders did
not differ significantly and were in the range of 2.24–
2.89%, hence it was not an influencing factor in some
variations in the ME values between the samples.
Studies have shown that a larger droplet size of the
emulsion generally results in higher free fat contents,
thus decreasing the ME value (Sheu and Rosenberg
1995, Hogan et al. 2001b, Tan et al. 2005). Young et al.
(1993b) showed that the ME values of spray dried
powders encapsulating anhydrous milk fat were inver-
sely proportional to the ratio of WPI-to-carbohydrate,
that is the free fat content decreased as the proportion
of WPI-to-carbohydrates decreased and also when a
mixture of WPI and carbohydrates was used as wall
materials other than WPI alone. In this study, such a
trend that could be attributed to either the emulsion
droplet size or the ratio of WPI to MD was not
obtained. The observed overall large free oil contents
were probably due to several combined factors
observed in this study other than a single factor, that
is (1) agglomeration and/or collapse of powder particles
that could alter their structural integrities and morpho-
logical structures, possibly resulting in a release of
encapsulated oil to the outside of the wall matrix due to
compression (Drusch et al. 2006), (2) large particle size
of emulsion oil droplets prior to spray drying and
(3) large vacuole volume which has been reported to be
positively related to free oil content (Keogh et al. 2001).
100
Bulk density
Bulk density of powders is affected by chemical
composition, particle size and moisture content as
well as by processing and storage conditions
(%  SD, w/w)
Microencapsulation
Moisture Free oil efficiency (ME)
2.24  0.89 13.44  4.13 59.62  12.40
2.56  0.62 11.88  0.66 59.52  2.25
2.47  0.99 15.75  0.38 44.52  1.33
2.89  0.74 11.39  1.28 66.18  3.82

(Beristain et al. 2001). In principle, density increases as
volume decreases at a given constant mass. In the
present study, the bulk densities of powders were
between 0.25–0.28 g cm3 and increased gradually as
the MD ratio increased (Table III). The higher densities
observed in the two samples (W50MD50 and
W10MD90) might be related to their high degree of
agglomeration and structural collapse (see Figure 4)
which could result in a subsequent decrease in volume
of the powder particles (Carolina et al. 2007) and a
more compact regular packing and arrangement of the
powder particles (Fuchs et al. 2006). The overall low
densities observed are assumed to be partly due to a
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large central vacuole found in the particles, as shown
in Figure 5.
Wettability
The ability of spray dried powders to mix with water or
other powders is one of the important physical proper-
ties related to reconstitution with water or dry blend
formulation. Wettability of powders is characterized as
the ability to rehydrate in water, that is the ability of a
bulk powder to absorb water (Gaiani et al. 2007).
In this study, the time taken for powders to disappear
For personal use only.
from the surface of water was used as a measure of the
degree of wettability (Table III). This measurement is
also denoted as sinkability (Fäldt and Bergenståhl
1996). The wetting times taken for the powders of W100
and W90MD10 were 18.05 and 12.09 min, respectively.
It was reduced remarkably to 9.06 and 7.61 min for the
W50MD50 and W10MD90 powders, respectively. This
indicates that MD having a more hydrophilic character
than does WPI increased hydrophilicity of the wall
systems, thus facilitating the accessibility and penetra-
tion of water into the powder particles. Moreover, the
same samples had higher densities which would have
increased their sinkablility in water. These results are in
agreement with several previous reports.
Agglomeration can increase the wettability of powders
because the liquid could more easily penetrate into the
pore system of the powder (Buffo et al. 2002).
Wettability depends on powder particle size, density,
porosity, surface charge, surface area, presence of
amphiphthic substances and surface activity of powders
(Vega and Roos 2006). It is important to note that the
wetting times observed in all samples, however, could
Table III. Bulk density and wettability of spray dried avocado oil powders at different ratios of
WPI-to-MD DE 5.
Powder wall system
W100
W90MD10
W50MD50
W10MD90
a,b,c,d
Different letters within each column are significantly different at p 5 0.05.
Microencapsulation of avocado oil by spray drying 555
have been delayed to some extent by the presence of the
substantial amounts of free oil.
Microstructural features
Representative SEM micrographs of the spray dried
powders are shown in Figures 4 and 5. In all cases, the
powders existed as a high degree of agglomerates of
small particles rather than as single discrete particles.
The state of agglomeration seemed to be more compact
and tightly bound with increasing the MD ratio in the
wall system. The size of powder particles was all in the
range of 1–10 mm. Agglomeration has been reported to
be partly related to the presence of a high level of
surface free fat (Hogan et al. 2001a, Vega and Roos
2006). The free oil contents of 11–16% may thus be
partly responsible to the observed powder particle
agglomeration. In all cases, no visible pores or cracks
were detected. Internal structures revealed the presence
of large sized vacuoles which is a common feature
typically observed in spray dried powders. No notice-
able differences in the internal structures between the
samples were detected.
The most pronounced structural difference between
the samples was surface topology, specifically the
presence or absence of surface depression (or collapse).
The powder particles of WPI only (i.e. W100) or in
combination with MD at 90 : 10 ratio (i.e. W90MD10)
were spherical and smooth with no significant surface
depression. Similar morphological shapes of whey
protein-based powders were also shown by other
studies (Al-Hakim and Stapley 2004,
Anandharamakrishnan et al. 2007). On the contrary,
the other two powders with the W50MD50 and
W10MD90 as wall systems exhibited a rather irregular
shape with deep surface depression being apparently
more evident with increasing the MD ratio in the
wall system. Other studies have also shown similar
surface topologies with surface depression or collapse
from spray dried particles containing MD as part
of wall materials (Soottitantawat et al. 2005,
Tewa-Tagne et al. 2007).
Surface depression or structural collapse and
agglomeration of powder particles have been
proposed to be related to glass transition and crystal-
lization of amorphous carbohydrate matrix of powder
particles (Roos and Karel 1991, Bhandari et al. 1997,
Bulk density (g cm3) Wettability (min g1)
0.2507  0.00004a 18.05  0.01a
0.2506  0.00007a 12.09  0.03b
0.2781  0.00008b 9.06  0.04c
0.2779  0.00008b 7.61  0.10d
 556 E. K. Bae & S. J. Lee
Journal of Microencapsulation Downloaded from informahealthcare.com by Columbia University on 04/05/13
For personal use only.
Figure 4. SEM micrographs of spray dried avocado oil encapsulated powders. Wall material systems: (a), (b) W100;
(c), (d) W90MD10; (e), (f) W50MD50; (g), (h) W10MD90.
Buffo et al. 2002, Le Meste et al. 2002, Velasco et al.
2003, Drusch et al. 2006, Carolina et al. 2007, Chiou
and Langrish 2007). At glass transition temperature,
surface droplet viscosity and stickiness of powder
particles increase, resulting in inter-particle bridge
formations that lead to caking and collapse of the
particles (Le Meste et al. 2002, Carolina et al. 2007).
Crystallization of amorphous carbohydrates is gener-
ally thought to occur during storage of powders rather
than during the spray drying since spray drying is very
rapid, thus forming amorphous particles (Chiou and
Langrish 2007). Glass transition temperature decreases
as moisture content increases (Roos and Karel 1991,
Avaltroni et al. 2004). This explains why crystallization
of powders normally takes place during storage,
especially at high relative humidity conditions. Studies
on drying temperatures and glass transition behaviour
showed that spray drying conditions above a glass
transition point could render amorphous particles very
sticky during the drying process (Bhandari et al. 1997).
Roos and Karel (1991) showed that MD with DE5 had
a glass transition temperature of 188 C and its glass
transition temperature decreased to 135, 90, 87, 58 and
44 C when its moisture content increased up to 1.9, 4.5,
 Microencapsulation of avocado oil by spray drying
Journal of Microencapsulation Downloaded from informahealthcare.com by Columbia University on 04/05/13
Figure 5. SEM micrographs of inner structures of spray dried avocado oil encapsulated powders. Wall material systems:
(a) W100; (b) W90MD10; (c) W50MD50; (d) W10MD90.
6.3, 8.9 and 10.6%, respectively, at relative humidity
For personal use only.
conditions of 11, 33, 43, 52 and 75, respectively. In this
study, the powder samples contained less than 3%
moisture in all cases and were stored at 4 C in air tight
glass bottles, thus agglomeration and collapse of the
powder particles observed in this study could be formed
during the spray drying process but one can not rule out
that it might happen upon spray drying or during
storage.
Oxidation of encapsulated avocado oil
The oxidative stability of avocado oils encapsulated in
the wall systems of WPI in combination with MD DE
5 at various different ratios was tested by measuring
their peroxide values (PVs) during storage of the
powders at 4 and 25 C for 8 weeks. It was also
analysed under the accelerated condition of 60 C
because low and ambient temperatures often require a
long period of time (Werman and Neerman 1987) which
was the case in this study. Unencapsulated avocado
bulk oil was also tested as a control under the same
conditions. The results are shown in Figure 6 (data for
4 C not shown). At day 0 before storage, all oil samples
had the initial PVs of 4.5 meq kg1 oil. No significant
differences were observed between the encapsulated and
control oils at day 0. This implies that lipid oxidation
did not occur during the encapsulation process (i.e.
emulsion preparation and spray drying). It was also
found that the PVs of all oil samples including the
unencapsulated control oil did not change during
storage of 8 weeks at both 4 and 25 C, suggesting
that, irrespective of microencapsulation, the cold
pressed crude avocado oil used in this study was very
557
stable against oxidation at both refrigerated and
ambient temperatures.
However, under the storage condition of 60 C, the
PVs were observed to start rising sharply in all cases
after 2 weeks. The increases continued until week 6 and
7 for the encapsulated oils and the control oil,
respectively, resulting in 7.3 and 8.2 meq kg1 oil,
respectively. Then the PVs of all oil samples decreased
slightly with time. At 60 C, the WPI-only wall system
reduced the oxidation rate of avocado oil slightly
compared to the control oil. The addition of MD with a
replacement of WPI in the wall system further slightly
improved the oxidative stability. This may be partly due
to the fact that oxygen is hydrophobic and the presence
of more hydrophilic MD could reduce oxygen perme-
ability of the wall matrix (Dzondo-Gadet 2005). Other
studies have shown that permeability of wall matrix to
oxygen is affected by wall matrix porosity and wall
matrix comprising of only protein has much higher
oxygen permeability than the wall matrix consisting of a
mixture of protein and small molecular weight carbo-
hydrates (Moreau and Rosenberg 1999, Kagami et al.
2003). The better oxidative stability with an addition of
MD with a higher DE value also contributed to its free
reducing groups acting as an antioxidant (Reineccius
2001, 2004). MDs with higher DE values have been
reported to provide better protection, in terms of
oxygen permeation, compared to MDs with lower
DE values (Reineccius 1991).
Taking account of all these possible effects, the
overall improvement on oxidative stability made by
encapsulation in this study seemed to be rather small,
unexpectedly. Irrespective of encapsulation, the overall
PV levels of 7–8 meq kg1 oil reached at 60 C after
 558 E. K. Bae & S. J. Lee

(a) 9
Bulk oil
8 W100

PV (meq peroxide/kg oil)

W90MD10
7 W50MD50
W10MD90
6

2
0 1 2 3 4 5 6 7 8 9
Storage time (weeks)
Journal of Microencapsulation Downloaded from informahealthcare.com by Columbia University on 04/05/13

(b) 9
Bulk oil
8 W100
PV (meq peroxide/kg oil)

W90MD10
7 W50MD50
W10MD90
6

2
For personal use only.

0 1 2 3 4 5 6 7 8 9
Storage time (weeks)

Figure 6. Changes in peroxide value (PV) during storage at 25 (a) and 60 C (b) for unencapsulated avocado bulk oil and spray
dried powder avocado oil encapsulated samples prepared at different ratios of WPI and MD DE5.

8 weeks reflected, as already indicated, that the cold
pressed crude avocado oil used was very stable, in terms
of oxidation, when stored under dark conditions.
Ramadan et al. (2003) reported that crude vegetable
oils are usually more stable than their corresponding
refined oils because of large amounts of natural
compounds (tocopherols, phospholipids, phytosterols
and phenols) that exhibit antioxidant activities which
are not present in refined oils. On the other hand, the
relatively high initial PVs observed in this study could
be because chlorophyll is present in a considerable
amount in crude avocado oil which can induce photo-
oxidation upon light exposure (Werman and Neerman
1987). In addition, some lipolytic enzymes, such as
lipases and lipoxigenases, released from fruit cells
during oil extraction procedure could also contribute
to the initial PV values to some extent (Elez-Martı́nez
et al. 2005).
increasing the MD ratio in the wall system, suggest-
ing that their physical properties can be tailored by
altering the ratio of wall materials of protein and
carbohydrates. At cold and ambient temperatures,
cold pressed avocado oil used in this study exhibited
a high oxidative stability, regardless of encapsulation.
This implies that spray dried cold pressed avocado oil
powders can have significant potential applications
for use in a variety of food and other non-food
products including cosmetic products, where a dry or
solid form of avocado oil is required. However, at
high temperature of 60 C, avocado oil underwent
oxidation significantly over time compared to the
samples stored at 4 and 25 C and encapsulation
conferred only a limited extent of protection. The
presence of high free oil content and the limited
extent of protection by encapsulation observed in this
study need to be further investigated.

Conclusions
Acknowledgements
Spray dried powders encapsulating avocado oil were
able to be produced using WPI and MD DE5 as wall This work was supported by the Korea Research
materials at various ratios. Physical properties, such Foundation Grant funded by the Korean Government
as wettability and density, were greatly improved by (MOEHRD) (KRF-2005-214-D00277).
 Microencapsulation of avocado oil by spray drying
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